CN103022457B - High-performance nano granular vanadium pentoxide lithium ion battery cathode material and preparation method thereof - Google Patents
High-performance nano granular vanadium pentoxide lithium ion battery cathode material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-performance nano granular vanadium pentoxide lithium ion battery cathode material and a preparation method thereof. Vanadium oxide or vanadium powder, a carbon nano tube, organic long-chain amine and hydrogen peroxide are taken as main raw materials; with a sol-gel method and under the hydrothermal condition, the long-chain amine and the carbon nano tube serve as templates and are subjected to post-sintering treatment to prepare the nano granular vanadium pentoxide; and the nano granular vanadium pentoxide can serve as a high-performance pentoxide lithium ion battery cathode material. The vanadium pentoxide nanoparticles have large specific surface areas, can increase active injection locations of the vanadium oxide material greatly, and meanwhile shorten the diffusion distances of lithium ions in the material to accelerate ion transport, so that the material can obtain large capacity and high power. Besides, the granular nano structure can effectively relieve the structure expansion/contraction caused when the lithium ions are injected or exit, so that the vanadium pentoxide nanoparticles also have good cycle performance.
Description
Technical field
The invention belongs to lithium ion battery field, be specifically related to granular vanadic oxide cathode material for lithium ion battery of a kind of high-performance nano and preparation method thereof.
Background technology
Along with scientific and technical development, people are increasing to the demand of the electronics energy.Lithium rechargeable battery is a kind of important electrical power storage equipment, and its utilization relates to the every aspect of our life.Especially in recent years,, along with the develop rapidly in the fields such as microelectronics industry, engineering in medicine, electric automobile, space technology, war industry, the range of application of lithium ion battery is more and more wider, also more and more higher to the requirement of performance of lithium ion battery.What the characteristic of lithium ion battery was strong depends on its electrode material, particularly cathode material, V
2o
5material, due to its special layer structure, makes it than other conventional cathode material (LiMn
2o
4, LiCoO
2and LiFePO
4deng) there is larger specific capacity.But due to the unsteadiness of its structure and intrinsic electronic conductivity and the problem such as ionic conductivity is low, make it be difficult to drop into business application.
According to many international and domestic pertinent literature reports, if can make vanadium oxide material nanometer, can well alleviate in charge and discharge process caused volumetric expansion/contraction problem when lithium ion embeds/deviates from, and then improve the structural stability of vanadium oxide material in electrochemical process.In addition, the vanadium oxide material of nanometer has very large surface activity area, can well fully contact with electrolyte, thereby the activity of increase lithium ion is injected position, improves the capacity of electrode material.The vanadium oxide particle of nanoscale, also can effectively shorten the diffusion length of lithium ion in material, and the transport velocity of lithium ion in electrode material accelerated, and is conducive to the high-power realization of electrode material.At present, the mode that realizes vanadium oxide material nanometer of reporting in document is a lot, as: EFI bundle method, ion sputtering method, reverse micelle method, electrodeposition process and physical/chemical vapour deposition process etc., but many conditions such as high temperature, high pressure and high vacuum that relate to, certain methods program comparision is loaded down with trivial details, and other certain methods need to adopt accurate complicated equipment.Vanadium oxide nanoparticle preparation method involved in the present invention, can be under the condition of gentleer and low power consuming, adopt simple technique, the vanadium oxide cathode material for lithium ion battery that persursor material synthesis of nano with low cost is granular, compares other manufacture crafts and has clear superiority.Prepared nano-granular vanadic oxide material, has superior chemical property, for the application of lithium ion battery provides more wide space.
At present, external existing employing vanadium source is the patent that raw material is prepared cathode material for lithium ion battery, is mainly by V
2o
5, V
2o
3vanadic salts react with lithium salts or other transition metal oxides as additive generate vanadium oxidate for lithium or other compounds as cathode material for lithium ion battery.If United States Patent (USP) (US5486346) is by M (NO
3)
2.6h
2o and LiOH, Li
2o, Li
2cO
3or Li (CH
3cOO) Li that prepared by reactant aqueous solution
xmO
2(wherein M is Ni or Co) particle, with V
2o
3, V
2o
5or NH
4vO
3at high temperature reaction obtains LiMVO
4as cathode material for lithium ion battery; European patent (EP0397608) is by V
2o
5with Li
2cO
3react the Li making through high-temperature fusion
1+xv
3o
8as cathode material for lithium ion battery.
Domestic about V
2o
5and composite material to do the patent of cathode material for lithium ion battery few in number.Chinese patent (97196288) is prepared chemical formula and is respectively Li
xm
yv
zo
(x+5z+ny)/2and M
yv
zo
(5z+ny)/2the vanadium metal oxide of amorphous state ternary thionate and the metal oxide of amorphous state binary nonthionate as lithium ion cathode materials; Chinese patent (0081943) uses vanadate to prepare vanadium oxide water and compositions as lithium ion cathode materials for raw material adopts the method for ion-exchange.
Also do not find with vanadium oxide or vanadium powder at present, hydrogen peroxide is raw material, and carbon nano-tube and organic long-chain amine are template, prepares the patent report of nano-granular vanadic oxide cathode material for lithium ion battery by Hydrothermal Synthesis and sintering reprocessing.
Summary of the invention
The object of the invention is taking vanadium oxide or vanadium powder, hydrogen peroxide as raw material, carbon nano-tube and organic long-chain amine are template, provide a kind of synthetic easy, with low cost, granular vanadic oxide cathode material for lithium ion battery of eco-friendly high-performance nano and preparation method thereof.
The granular vanadic oxide cathode material for lithium ion battery of high-performance nano that the present invention proposes, this battery cathode material is taking carbon nano-tube and organic long-chain amine as template in hydro-thermal situation, obtain through the preparation of temperature control sintering processes, its pattern is the nutty structure of nanoscale, nanometer vanadic oxide particle size is at 100-300nm, the content of the relative vanadium oxide of carbon nano-tube or vanadium powder is 5.5wt%～20wt%, and the content of the relative vanadium oxide of organic long-chain amine or vanadium powder is 15.5wt%～50wt%.
In the present invention, described organic long-chain amine be in lauryl amine, tetradecy lamine or cetylamine any.
The preparation method of the granular vanadic oxide cathode material for lithium ion battery of high-performance nano that the present invention proposes, concrete steps are as follows:
(1) vanadium oxide or vanadium powder are mixed with 30% hydrogen peroxide, after vigorous reaction, form vanadium oxide colloidal sol; Wherein: vanadium oxide or vanadium powder and concentration are that the mass volume ratio of 30% hydrogen peroxide is 1:8-1:60 (g/ml);
(2) carbon nano-tube disperseed and wash to neutral;
(3) carbon nano-tube step (2) being obtained and organic long-chain amine join in the vanadium oxide colloidal sol that step (1) obtains and fully stir, until form the gluey suspension-turbid liquid of black;
(4) gluey black suspension-turbid liquid is moved into hydrothermal reaction kettle, then reactor is placed in to temperature control box, through 1-10 days hydro-thermal reactions, obtain black precipitate;
(5) gained black precipitate is carried out under air atmosphere to sintering processes, obtain end product.
In the present invention, described in step (2), carbon nano-tube is multi-walled carbon nano-tubes or Single Walled Carbon Nanotube.
In the present invention, in step (2), carbon nano-tube is disperseed, concrete steps are: in the nitration mixture that the carbon nano-tube input concentrated sulfuric acid and red fuming nitric acid (RFNA) volume ratio are 1:1-6:1, and under 30-60 DEG C of water-bath sonic oscillation 1-5 hour, then by gained carbon nano-tube water and alcohol blend washing to neutral.
In the present invention, the organic long-chain amine described in step (3) be in lauryl amine, tetradecy lamine or cetylamine any.
In the present invention, in step (4), controlling hydrothermal reaction kettle temperature is 80-300 DEG C.
In the present invention, the sintering temperature in step (5) under air atmosphere is 250-650 DEG C.
In the present invention, described vanadium oxide colloidal sol adopts sol-gel process preparation, mix by mass volume ratio 1:8-1:60 (g/ml) with hydrogen peroxide (concentration is 30%) by vanadium oxide or vanadium powder, this reaction is a very exothermic the process of emitting oxygen, just obtains subsequently orange-red vanadium oxide colloidal sol.
The present invention is taking vanadium oxide or vanadium powder, hydrogen peroxide as raw material, and carbon nano-tube and organic long-chain amine are template, prepare a kind of nano level vanadic oxide particle as cathode material for lithium ion battery through hydro-thermal and sintering processes.Have simple to operate, with low cost, eco-friendly feature.Nano-granular vanadic oxide, as cathode materials for lithium battery, has the high power capacity of the theoretical value of approaching and good cycle performance and large high rate performance.These good performances all have benefited from the nano-granular structure of vanadic oxide.
The nano-granular vanadic oxide of synthesized of the present invention has embodied the peculiar property that nanoscale material has aspect electrochemistry: large active surface area, can fully contact with electrolyte, and increase the active position of injecting of lithium ion, improve the capacity of electrode material; Nano-granular structure can be accelerated lithium ion transporting and effectively having alleviated in electrochemical process the caused material volume of lithium ion deintercalation and change therein, thereby has improved large multiplying power and the cycle performance of vanadium oxide material.
Brief description of the drawings
Fig. 1 is the SEM(ESEM of the vanadic oxide nanoparticle prepared of the present invention) figure.
Fig. 2 is the XRD(X x ray diffraction of the vanadic oxide nanoparticle prepared of the present invention) figure.
Fig. 3 under different charge-discharge magnifications, the cycle performance figure (voltage range 1.5-4V) of vanadic oxide nanoparticle during as cathode material for lithium ion battery.
Embodiment
Below by example and accompanying drawing, the present invention is specifically described and is illustrated, it is important to point out that the present embodiment, only for the present invention is further detailed, can not be interpreted as limiting the scope of the invention.
Embodiment 1:
One, the preparation of vanadium oxide colloidal sol
Adopt sol-gel process to prepare vanadium oxide colloidal sol, by 1gV
2o
5powder and hydrogen peroxide (30% concentration), stir at 5 DEG C of water-bath lower magnetic forces than mixing with the mass/volume of 1:10 (g/ml), will be accompanied by violent oxygen and heat release, about 1 hour of the whole process of putting soon afterwards.Finally generate orange-red vanadium oxide colloidal sol.
Two, the dispersion of carbon nano-tube
Getting original carbon nano-tube 1g, to add 50mL volume ratio be in the concentrated sulfuric acid/red fuming nitric acid (RFNA) of 1:1, sonic oscillation 1 hour under 35 DEG C of water-baths.After cooling, within centrifugal 10 minutes, go out upper strata nitration mixture with 1000 revs/min, then filter, washing is to neutral.
Three, the preparation of black colloidal suspension-turbid liquid
The vanadium oxide colloidal sol of preparation is mixed to rear magnetic agitation～1 hour mutually with scattered 0.08g carbon nano-tube and 0.2g lauryl amine, until form the gluey suspension-turbid liquid of black.
Four, under hydrothermal condition, prepare black powder shape product
Gluey black turbid liquid is moved in hydrothermal reaction kettle and carries out 2 days 100 DEG C of hydro-thermal reactions.Gained sediment is through alcohol immersion, washing and after filtering, and 100 DEG C of vacuumize 8 hours, obtains black powder shape product.
Five, sintering obtains the vanadic oxide cathode material of Nanoparticulate
Gained black powder shape product is placed in to Muffle furnace, under air atmosphere, after 350 DEG C of sintering, obtains pale yellow powder product, be the vanadic oxide cathode material of Nanoparticulate.Scanning Electron Microscope photos reveal (Fig. 1): final products therefrom is the nano particle being cross-linked with each other, and size is between 100-300nm.
Embodiment 2:
One, the preparation of vanadium oxide colloidal sol
Adopt sol-gel process to prepare vanadium oxygen colloidal sol, by 1gV
2o
3powder and hydrogen peroxide (30% concentration), stir at 5 DEG C of water-bath lower magnetic forces than mixing with the mass/volume of 1:25 (g/ml), will be accompanied by violent oxygen and heat release, about 1 hour of the whole process of putting soon afterwards.Finally generate orange-red vanadium oxide colloidal sol.
Two, the dispersion of carbon nano-tube
Getting original carbon nano-tube 1g, to add 50mL volume ratio be in the concentrated sulfuric acid/red fuming nitric acid (RFNA) of 2:1, sonic oscillation 2.5 hours under 40 DEG C of water-baths.After cooling, within centrifugal 10 minutes, go out upper strata nitration mixture with 1000 revs/min, then filter, washing is to neutral.
Three, the preparation of black colloidal suspension-turbid liquid
The vanadium oxide colloidal sol of preparation is mixed to rear magnetic agitation～1 hour mutually with scattered 0.12g carbon nano-tube and 0.3g lauryl amine, until form the gluey suspension-turbid liquid of black.
Four, under hydrothermal condition, prepare black powder shape product
Gluey black turbid liquid is moved in hydrothermal reaction kettle and carries out 4 days 150 DEG C of hydro-thermal reactions.Gained sediment is through alcohol immersion, washing and after filtering, and 100 DEG C of vacuumize 8 hours, obtains black powder shape product.
Five, sintering obtains the vanadic oxide cathode material of Nanoparticulate
Gained black powder shape product is placed in to Muffle furnace, under air atmosphere, after 400 DEG C of sintering, obtains pale yellow powder product, be the vanadic oxide cathode material of Nanoparticulate.Scanning Electron Microscope photos reveal (Fig. 1): final products therefrom is the nano particle being cross-linked with each other, and size is between 100-300nm.
Embodiment 3:
One, the preparation of vanadium oxide colloidal sol
Adopt sol-gel process to prepare vanadium oxide colloidal sol, 1g vanadium powder and hydrogen peroxide (30% concentration) are mixed with the mass/volume ratio of 1:35 (g/ml), stir at 5 DEG C of water-bath lower magnetic forces, will be accompanied by violent oxygen and heat release, about 1 hour of the whole process of putting soon afterwards.Finally generate orange-red vanadium oxide colloidal sol.
Two, the dispersion of carbon nano-tube
Getting original carbon nano-tube 1g, to add 50mL volume ratio be in the concentrated sulfuric acid/red fuming nitric acid (RFNA) of 2.5:1, sonic oscillation 3 hours under 45 DEG C of water-baths.After cooling, within centrifugal 10 minutes, go out upper strata nitration mixture with 1000 revs/min, then filter, washing is to neutral.
Three, the preparation of black colloidal suspension-turbid liquid
The vanadium oxide colloidal sol of preparation is mixed to rear magnetic agitation～1 hour mutually with scattered 0.15g carbon nano-tube and 0.35g lauryl amine, until form the gluey suspension-turbid liquid of black.
Four, under hydrothermal condition, prepare black powder shape product
Gluey black turbid liquid is moved in hydrothermal reaction kettle and carries out 6 days 200 DEG C of hydro-thermal reactions.Gained sediment is through alcohol immersion, washing and after filtering, and 100 DEG C of vacuumize 8 hours, obtains black powder shape product.
Five, sintering obtains the vanadic oxide cathode material of Nanoparticulate
Gained black powder shape product is placed in to Muffle furnace, under air atmosphere, after 450 DEG C of sintering, obtains pale yellow powder product, be the vanadic oxide cathode material of Nanoparticulate.Scanning Electron Microscope photos reveal (Fig. 1): final products therefrom is the nano particle being cross-linked with each other, and size is between 100-300nm.
Embodiment 4:
One, the preparation of vanadium oxide colloidal sol
Adopt sol-gel process to prepare vanadium oxygen colloidal sol, by 1gVO
2powder and hydrogen peroxide (30% concentration), stir at 5 DEG C of water-bath lower magnetic forces than mixing with the mass/volume of 1:55 (g/ml), will be accompanied by violent oxygen and heat release, about 1 hour of the whole process of putting soon afterwards.Finally generate orange-red vanadium oxide colloidal sol.
Two, the dispersion of carbon nano-tube
Getting original carbon nano-tube 1g, to add 50mL volume ratio be in the concentrated sulfuric acid/red fuming nitric acid (RFNA) of 5:1, sonic oscillation 4 hours under 55 DEG C of water-baths.After cooling, within centrifugal 10 minutes, go out upper strata nitration mixture with 1000 revs/min, then filter, washing is to neutral.
Three, the preparation of black colloidal suspension-turbid liquid
The vanadium oxide colloidal sol of preparation is mixed to rear magnetic agitation～1 hour mutually with scattered 0.2g carbon nano-tube and 0.45g lauryl amine, until form the gluey suspension-turbid liquid of black.
Four, under hydrothermal condition, prepare black powder shape product
Gluey black turbid liquid is moved in hydrothermal reaction kettle and carries out 8 days 240 DEG C of hydro-thermal reactions.Gained sediment is through alcohol immersion, washing and after filtering, and 100 DEG C of vacuumize 8 hours, obtains black powder shape product.
Five, sintering obtains the vanadic oxide cathode material of Nanoparticulate
Gained black powder shape product is placed in to Muffle furnace, under air atmosphere, after 550 DEG C of sintering, obtains pale yellow powder product, be the vanadic oxide cathode material of Nanoparticulate.Scanning Electron Microscope photos reveal (Fig. 1): final products therefrom is the nano particle being cross-linked with each other, and size is between 100-300nm.
Pattern and the structure of gained nano-granular vanadic oxide have been characterized with scanning electron microscopy (SEM, Philips-XL-30FEG) figure and X-ray diffraction (XRD) figure.Using lithium metal as to electrode and reference electrode, contain 1M/LLiPF
6ethylene carbonate (EC) and methyl ethyl carbonate (EMC) mixed solution (Samsung of Korea S provides) be electrolyte, wherein EC: EMC=1: 1, carry out the assembling of battery in mutually at the gloves that are full of argon gas.Adopt electrochemical analyser CHI660C (Chenghua, Shanghai) to carry out charge-discharge test.
Being prepared as follows of work electrode:
70% nano-granular vanadic oxide is mixed with 20% carbon black, adds 10%PVDF(as binder), more slowly add 1-Methyl-2-Pyrrolidone, until Sample Dilution is also fully stirred into pasty state.Again it is applied uniformly on aluminium foil.The oven dry aluminium foil of slowly heating, first 40
oc heating 1 hour, then 80
oc heating 1 hour, finally with 120
oc vacuumize 8 hours.Then naturally cool to room temperature.
SEM figure and the XRD of gained nano-granular vanadic oxide scheme as depicted in figs. 1 and 2, and its charge-discharge performance figure as shown in Figure 3.Vanadic oxide prepared by known the inventive method is nano-granular, belongs to orthorhombic structure.It shows good chemical property during as cathode material for lithium ion battery: low range discharges and recharges down (150mA/g), and capacity has exceeded 400mAh/g first, after 50 circulations, still keeps specific capacity more than 200mAh/g; Under high power charging-discharging (300mA/g), although capacity reduces (approximately 385mAh/g) to some extent first, after 50 circulations, also there is the specific capacity that approaches 200 mAh/g.Visible, the granular vanadic oxide cathode material of high-performance nano has high power capacity (specific capacity of conventional cathode material is between 140-160 mAh/g), good circulation and high-power feature.
Above-described embodiment is only in order to illustrate technological thought of the present invention and feature; its object is to make those of ordinary skill in the art can understand content of the present invention and implement according to this; the scope of this patent is also not only confined to above-mentioned specific embodiment; be all equal variation or modifications of doing according to disclosed method, be still encompassed in protection scope of the present invention.
Claims (6)
1. the granular vanadic oxide cathode material for lithium ion battery of high-performance nano, it is characterized in that this battery cathode material is taking carbon nano-tube and organic long-chain amine as template in hydro-thermal situation, obtain through the preparation of temperature control sintering processes, its pattern is the nutty structure of nanoscale, nanometer vanadic oxide particle size is at 100-300nm, the content of the relative vanadium oxide of carbon nano-tube or vanadium powder is 5.5wt%～20wt%, and the content of the relative vanadium oxide of organic long-chain amine or vanadium powder is 15.5wt%～50wt%; Described nano-granular vanadic oxide cathode material for lithium ion battery prepares by following method, and concrete steps are as follows:
(1) vanadium oxide or vanadium powder are mixed with 30% hydrogen peroxide, after vigorous reaction, form vanadium oxide colloidal sol; Wherein: vanadium oxide or vanadium powder and concentration are that the mass volume ratio of 30% hydrogen peroxide is 1:8-1:60 (g/ml);
(2) carbon nano-tube disperseed and wash to neutral;
(3) carbon nano-tube step (2) being obtained and organic long-chain amine join in the vanadium oxide colloidal sol that step (1) obtains and fully stir, until form the gluey suspension-turbid liquid of black;
(4) gluey black suspension-turbid liquid is moved into hydrothermal reaction kettle, then reactor is placed in to temperature control box, through 1-10 days hydro-thermal reactions, obtain black precipitate; Controlling hydrothermal reaction kettle temperature is 80-300 DEG C;
(5) gained black precipitate is carried out under air atmosphere to sintering processes, the sintering temperature under air atmosphere is 250-650 DEG C, obtains end product.
2. the granular vanadic oxide cathode material for lithium ion battery of high-performance nano according to claim 1, it is characterized in that organic long-chain amine be in lauryl amine, tetradecy lamine or cetylamine any.
3. a preparation method for the granular vanadic oxide cathode material for lithium ion battery of high-performance nano as claimed in claim 1, is characterized in that concrete steps are as follows:
(1) vanadium oxide or vanadium powder are mixed with 30% hydrogen peroxide, after vigorous reaction, form vanadium oxide colloidal sol; Wherein: vanadium oxide or vanadium powder and concentration are that the mass volume ratio of 30% hydrogen peroxide is 1:8-1:60 (g/ml);
(2) carbon nano-tube disperseed and wash to neutral;
(3) carbon nano-tube step (2) being obtained and organic long-chain amine join in the vanadium oxide colloidal sol that step (1) obtains and fully stir, until form the gluey suspension-turbid liquid of black;
(4) gluey black suspension-turbid liquid is moved into hydrothermal reaction kettle, then reactor is placed in to temperature control box, through 1-10 days hydro-thermal reactions, obtain black precipitate; Controlling hydrothermal reaction kettle temperature is 80-300 DEG C;
(5) gained black precipitate is carried out under air atmosphere to sintering processes, the sintering temperature under air atmosphere is 250-650 DEG C, obtains end product.
4. preparation method according to claim 3, is characterized in that described in step (2), carbon nano-tube is multi-walled carbon nano-tubes or Single Walled Carbon Nanotube.
5. preparation method according to claim 3, it is characterized in that in step (2), carbon nano-tube is disperseed, concrete steps are: in the nitration mixture that the carbon nano-tube input concentrated sulfuric acid and red fuming nitric acid (RFNA) volume ratio are 1:1-6:1, and under 30-60 DEG C of water-bath sonic oscillation 1-5 hour, then by gained carbon nano-tube water and alcohol blend washing to neutral.
6. preparation method according to claim 3, it is characterized in that the organic long-chain amine described in step (3) be in lauryl amine, tetradecy lamine or cetylamine any.
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| WO2015178790A1 (en) * | 2014-05-21 | 2015-11-26 | Общество с ограниченной ответственностью "Литион" | Electrode for an electrical current source and method for the production thereof |
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| CN106410178B (en) * | 2016-11-30 | 2019-04-26 | 武汉理工力强能源有限公司 | A kind of preparation method and application of mesoporous vanadic anhydride micron ball |
| CN108899534B (en) * | 2018-06-19 | 2021-03-16 | 清华大学 | Preparation method of vanadium oxide as positive electrode material of lithium ion battery capacitor |
| CN109775758A (en) * | 2018-12-26 | 2019-05-21 | 中国电子科技集团公司第十八研究所 | Preparation method of large-layer-spacing vanadium pentoxide |
| CN115072779B (en) * | 2022-06-08 | 2023-11-28 | 攀钢集团攀枝花钢铁研究院有限公司 | Lithium ion battery anode material V 2 O 5 Preparation method of nanotube and lithium ion button cell thereof |
| CN115064684B (en) * | 2022-07-18 | 2024-01-23 | 宁波烯固数造电池科技有限公司 | Vanadium oxide/reduced graphene oxide composite material and preparation method and application thereof |
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| CN101767771A (en) * | 2010-01-08 | 2010-07-07 | 武汉理工大学 | Preparation method of vanadium oxide/carbon nanometer tube composite materials with interpenetrating network structures |
| CN102795666A (en) * | 2012-07-27 | 2012-11-28 | 中南大学 | Method for preparing vanadium pentoxide cathode nano-material of lithium-ion battery |
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| CN101767771A (en) * | 2010-01-08 | 2010-07-07 | 武汉理工大学 | Preparation method of vanadium oxide/carbon nanometer tube composite materials with interpenetrating network structures |
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