CN108735987B - Tin-vanadium-cobalt-manganese composite oxide nano-particles and preparation method thereof - Google Patents
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Abstract
The invention discloses a tin-vanadium-cobalt-manganese composite oxide nanoparticle and a preparation method thereof, wherein a certain amount of manganese acetate, cobalt acetate, vanadium acetylacetonate and dibutyltin oxalate are dissolved in a certain volume of N, N-dimethylformamide and ethanol, then a proper amount of polyvinylpyrrolidone is added, and stirring is carried out to obtain a brownish red precursor mixture solution; then electrostatic spinning is carried out under certain voltage, flow rate and relative humidity atmosphere; and then sintering the electrostatic spinning product to obtain the tin-vanadium-cobalt-manganese composite oxide nano-particles. Electrochemical experiments prove that the tin-vanadium-cobalt-manganese composite oxide nano-particles prepared by the method have wide application prospects as a lithium ion battery cathode material. In the whole preparation process, the operation is simple, the raw material cost is low, the equipment investment is low, and the method is suitable for batch production.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to a tin-vanadium-cobalt-manganese composite oxide nanoparticle and a preparation method thereof.
Background
The nano materials have a series of characteristics, such as quantum size effect, small size effect, surface effect and quantum tunneling effect, so that the nano materials are obviously different from macroscopic characteristics in the aspects of light, electricity, magnetism, heat, sound, superconduction and the like, and have a background of wide application in the aspects of magnetic materials, electronic materials, optical materials, novel batteries and the like.
The nano material also has the characteristics of large specific surface area, high surface activity, short ion diffusion path, strong peristalsis, high plasticity and the like, and the application of the nano material to the electrode material of the lithium ion battery can obviously improve the extraction/insertionLithium capacity and extended cycle life of the electrode and improved wettability of the electrode material with the electrolyte solution (Lihong et al, lithium ion battery nanomaterial research, electrochemistry, 2000,6(2): 131-. The tin-based negative electrode material has higher theoretical specific capacity, lower lithium intercalation potential in the charging and discharging process, no solvent co-intercalation problem, good safety performance and higher volumetric specific energy and mass specific energy, so that materials such as tin oxide, tin-based composite oxide and the like are more and more concerned (Wu Guaiang et al, the current situation and development of the negative electrode material of the lithium ion battery, battery 2001,31, 54-57). Tin oxide SnOXAlthough the lithium ion battery has high reversible lithium intercalation capacity, the first irreversible capacity is high, and the cycle performance is poor. (V) of vanadate CompoundxOy) Usually form a layered structure, very beneficial to Li+Due to the characteristic of vanadate insolubility in electrolyte solution. Therefore, due to the excellent electrochemical performance of vanadate, the vanadate has been considered as a lithium battery material and has been paid attention in recent years. In 2014, li soldiers and the like adopt a hydrothermal method to prepare monodisperse M-phase vanadium dioxide nanoparticles (a preparation method of the monodisperse M-phase vanadium dioxide nanoparticles, with the publication number of CN 104071843A). However, during the cyclic phase transition of the vanadate compound to remove Li, irreversible phase transition thereof causes the deterioration of the charge/discharge capacity, resulting in a capacity loss (Jin K et al, Journal of power sources,1999,83(1), 79-83). At present, cobalt-based positive electrode materials and modified materials thereof are still dominant in the market. In 2014, Wangcheng et al prepared cobaltosic oxide spherical particles for a positive electrode material of a lithium ion battery by using a hydrothermal method and discussed the electrochemical performance (Wangcheng et al, research on a production process of battery-grade cobaltosic oxide, a metal functional material, 2014,21(2): 36-40). But the thermal stability of the material is still to be improved. For manganese series materials, the manganese source active MnO can be used for preparing spinel type lithium manganate2、Mn2O3、Mn3O4、MnCO3Of iso-manganeseA compound is provided. In 2006, Fang et al prepared LiNi by a ball milling method0.5Mn1.5O4And the charge-discharge cycle performance of the material after being prepared into the lithium ion battery is researched (Fang et al, Mater Lett.,2006,60(9-10): 1273-. Manganese sulfate is used as a raw material by Chenlijuan and the like, and a trimanganese tetroxide product is prepared by adopting a forced air oxidation method (Chenlijuan and the like, preparation research and application of trimanganese tetroxide for a lithium secondary battery anode material, 2012,41(3): 473-. However, the manganate used as a lithium ion battery material has the problems of unsatisfactory cycle use frequency and the like in the application aspect. In order to further improve the electrochemical performance of the lithium ion battery, the invention adopts the electrostatic spinning technology to prepare the tin-vanadium-cobalt-manganese composite oxide (SnO)2/VO2/CoO/Mn3O4) And (3) nanoparticles.
Disclosure of Invention
The invention aims to solve the technical problem of providing a tin-vanadium-cobalt-manganese composite oxide (SnO)2/VO2/CoO/Mn3O4) Nanoparticles and a method for preparing the same.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of tin-vanadium-cobalt-manganese composite oxide nanoparticles comprises the steps of taking manganese acetate, cobalt acetate, vanadium acetylacetonate and dibutyltin oxalate as main raw materials, adding a proper amount of high molecules as an adhesive, preparing an electrostatic spinning product by using an electrostatic spinning technology under the condition of high voltage, and sintering in a muffle furnace to obtain the tin-vanadium-cobalt-manganese composite oxide (SnO)2/VO2/CoO/Mn3O4) The nanoparticle specifically comprises the following steps:
1) weighing a certain amount of manganese acetate (Mn (CH)3COO)2) Cobalt acetate (Co (CH)3COO)2) Vanadium (C) acetylacetonate15H21O6V), dibutyl tin oxalate (C)12H24O4Sn) dissolved in a volume of N, N-Dimethylformamide (DMF) and ethanol (CH)3CH2OH), then adding a proper amount of polymer which is a binding agent PVP (K-120, polyvinylpyrrolidone),stirring for 6-12 h to obtain a brownish red precursor mixture solution, wherein the molar ratio of metal elements in the mixture solution is Mn: co: v: sn is 3: 1: 1: 1; 2) performing electrostatic spinning on the brownish red precursor mixture solution under the conditions of 18-20 kv voltage, 0.8-1.0 mL/h flow rate and relative humidity of 30-40%;
3) placing the obtained electrostatic spinning product in a crucible, then placing the crucible in a muffle furnace at 800-900 ℃ for sintering for 5-7h, and then naturally cooling to room temperature to obtain the tin-vanadium-cobalt-manganese composite oxide SnO2/VO2/CoO/Mn3O4And (3) nanoparticles.
The invention also provides application of the tin vanadium cobalt manganese composite oxide nano-particles obtained by the preparation method, and the nano-particles are used as a lithium ion battery cathode material and have the specific discharge capacity of 478.7mAh g for the first time-1And the charging and discharging specific capacity is kept at 390mAh g after the circulation for 85 times-1Above, the charge and discharge efficiency is still maintained above 99% after 85 times of circulation.
Compared with the prior art, the invention has the following characteristics:
the invention prepares a tin vanadium cobalt manganese composite oxide (SnO)2/VO2/CoO/Mn3O4) The nano-particles have excellent performance, and the charge-discharge test shows that the first discharge specific capacity of the nano-particles as the battery cathode material is 478.7mAh g-1And the charging and discharging specific capacity is kept at 390mAh g after the circulation for 85 times-1Above, the charge-discharge efficiency remained above 99% after 85 cycles (fig. 3).
Drawings
FIG. 1 is an XRD diagram of the tin vanadium cobalt manganese composite oxide nanoparticles prepared by the invention;
FIG. 2 is an SEM image of the tin vanadium cobalt manganese composite oxide nanoparticles prepared by the invention;
FIG. 3 is a diagram of the electrochemical performance of the tin vanadium cobalt manganese composite oxide nanoparticles prepared by the present invention as a battery material.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
3.0mmol (0.519g) of manganese acetate (Mn (CH) was weighed3COO)2) 1.0mmol (0.177g) of cobalt acetate (Co (CH)3COO)2) 1.0mmol (0.348g) of vanadium acetylacetonate (C)15H21O6V) and 1.0mmol (0.351g) of dibutyltin oxalate (C)12H24O4Sn) is dissolved in 10mL of N, N-Dimethylformamide (DMF) and 10mL of ethanol, then 3.0g of PVP (K-120, polyvinylpyrrolidone) is added, and stirring is carried out for 6h, so as to obtain a brownish red precursor mixture solution; carrying out electrostatic spinning on the brownish red precursor mixture solution under the conditions of 18kv voltage, 0.8mL/h flow rate and relative humidity of 30%; and (3) placing the obtained electrostatic spinning product in a crucible, then placing the crucible in a muffle furnace to sinter for 5 hours at 800 ℃, and then naturally cooling to room temperature to obtain the tin-vanadium-cobalt-manganese composite oxide nano-particles. Performing powder X-ray diffraction analysis (figure 1) on the obtained tin-vanadium-cobalt-manganese composite oxide nanoparticles to determine that the structural formula of the composite oxide is SnO2/VO2/CoO/Mn3O4The morphology of the particles was observed to be nanoparticle-shaped by SEM (FIG. 2), and the properties were measured by an electrochemical tester (FIG. 3).
Example 2
1.5mmol (0.260g) of manganese acetate (Mn (CH) was weighed3COO)2) 0.5mmol (0.0885g) of cobalt acetate (Co (CH)3COO)2) 0.5mmol (0.174g) of vanadium acetylacetonate (C)15H21O6V) and 0.5mmol (0.176g) of dibutyltin oxalate (C)12H24O4Sn) in 10mL of N, N-Dimethylformamide (DMF) and 10mL of ethanol (CH)3CH2OH), then adding 2.5g of PVP (K-120, polyvinylpyrrolidone), and stirring for 12h to obtain a brownish red precursor mixture solution; carrying out electrostatic spinning on the brownish red precursor mixture solution under the conditions of 19kv voltage, 0.9mL/h flow rate and 35% relative humidity; placing the obtained electrostatic spinning product in a crucible, then placing the crucible in a muffle furnace to sinter for 6h at 850 ℃, and then naturally cooling to room temperature to obtain the tin-vanadium-cobalt-manganese composite oxide (SnO)2/VO2/CoO/Mn3O4) And (3) nanoparticles. And performing powder X-ray diffraction analysis and scanning electron microscope SEM test on the obtained tin-vanadium-cobalt-manganese composite oxide nanoparticles, and testing the cycle performance and the charge and discharge performance of the tin-vanadium-cobalt-manganese composite oxide nanoparticles by using an electrochemical tester.
Example 3
3.0mmol (0.519g) of manganese acetate (Mn (CH) was weighed3COO)2) 1.0mmol (0.177g) of cobalt acetate (Co (CH)3COO)2) 1.0mmol (0.348g) of vanadium acetylacetonate (C)15H21O6V) and 1.0mmol (0.351g) of dibutyltin oxalate (C)12H24O4Sn) in 10mL of N, N-Dimethylformamide (DMF) and 10mL of ethanol (CH)3CH2OH), then adding 3.2g of PVP (K-120, polyvinylpyrrolidone) and stirring for 8 hours to obtain a brownish red precursor mixture solution; carrying out electrostatic spinning on the brownish red precursor mixture solution under the conditions of 20kv voltage, 1.0mL/h flow rate and 40% relative humidity; placing the obtained electrostatic spinning product in a crucible, then placing the crucible in a muffle furnace to sinter at 900 ℃ for 7h, and then naturally cooling to room temperature to obtain the tin-vanadium-cobalt-manganese composite oxide (SnO)2/VO2/CoO/Mn3O4) And (3) nanoparticles. And performing powder X-ray diffraction analysis and scanning electron microscope SEM test on the obtained tin-vanadium-cobalt-manganese composite oxide nanoparticles, and testing the cycle performance and the charge and discharge performance of the tin-vanadium-cobalt-manganese composite oxide nanoparticles by using an electrochemical tester.
Claims (2)
1. The preparation method of the tin vanadium cobalt manganese composite oxide nano-particles is characterized in that the chemical formula of the tin vanadium cobalt manganese composite oxide nano-particles is SnO2/VO2/CoO/Mn3O4The preparation method comprises the following steps:
1) weighing a certain amount of manganese acetate, cobalt acetate, vanadium acetylacetonate and dibutyltin oxalate, dissolving the manganese acetate, the cobalt acetate, the vanadium acetylacetonate and the dibutyltin oxalate in a certain volume of N, N-dimethylformamide and ethanol, adding a proper amount of polyvinylpyrrolidone K-120, and stirring for 6-12 h to obtain a brownish red precursor mixture solution, wherein the molar ratio of metal elements in the mixture solution is Mn: co: v: sn is 3: 1: 1: 1;
2) performing electrostatic spinning on the obtained brownish red precursor mixture solution under the conditions of 18-20 kv voltage, 0.8-1.0 mL/h flow rate and relative humidity of 30-40%;
3) and placing the obtained electrostatic spinning product in a crucible, then placing the crucible in a muffle furnace to sinter for 5-7h at 800-900 ℃, and then naturally cooling to room temperature to obtain the tin-vanadium-cobalt-manganese composite oxide nano-particles.
2. The use of the tin vanadium cobalt manganese composite oxide nanoparticles prepared by the preparation method according to claim 1, wherein the tin vanadium cobalt manganese composite oxide nanoparticles are used as a negative electrode material of a lithium ion battery, and the first discharge specific capacity of the tin vanadium cobalt manganese composite oxide nanoparticles is 478.7mAh g-1And the charging and discharging specific capacity is kept at 390mAh g after the circulation for 85 times-1Above, the charge and discharge efficiency is still maintained above 99% after 85 times of circulation.
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| CN101770868A (en) * | 2009-01-06 | 2010-07-07 | 中国科学院化学研究所 | Compound of metal/metal oxide and preparation method and application thereof |
| KR20140036660A (en) * | 2012-09-17 | 2014-03-26 | (주)오렌지파워 | Active material for anode, method of fabricating the same and battery having the same |
| CN105514369A (en) * | 2015-12-07 | 2016-04-20 | 南京师范大学 | Hollow SnO2/Co3O4 hybrid nanotube as well as preparation method and application thereof |
| JP2018041536A (en) * | 2016-09-05 | 2018-03-15 | セイコーエプソン株式会社 | Secondary battery, method for manufacturing secondary battery, and electronic device |
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