CN103022457A - 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 the 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 the development of science and technology, 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, and is also more and more higher to the requirement of performance of lithium ion battery.The characteristic of lithium ion battery is strong depends on its electrode material, particularly cathode material, V
2O
5Material is because its special layer structure makes it than other conventional cathode material (LiMn
2O
4, LiCoO
2And LiFePO
4Deng) have a larger specific capacity.But because the problem such as the unsteadiness of its structure and intrinsic electronic conductivity and ionic conductivity be low makes it be difficult to drop into commercial the application.
According to many international and domestic pertinent literature reports, if can make the vanadium oxide material nanometer, can alleviate well that lithium ion embeds in the charge and discharge process/caused volumetric expansion/contraction problem when deviating 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 that increases lithium ion is injected the 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, so that the transport velocity of lithium ion in electrode material accelerated, is conducive to the high-power realization of electrode material.At present, the mode of the realization vanadium oxide material nanometer of reporting in the 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, the 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 gentleness 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 is compared other manufacture crafts and is had 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 prepares cathode material for lithium ion battery, mainly is with V
2O
5, V
2O
3Or the vanadium oxidate for lithium that generates as additive and lithium salts or the reaction of other transition metal oxides of vanadic salts or other compounds are as cathode material for lithium ion battery.Such as United States Patent (USP) (US5486346) with M (NO
3)
2.6H
2O and LiOH, Li
2O, Li
2CO
3Or Li (CH
3COO) Li of reactant aqueous solution preparation
xMO
2(wherein M is Ni or Co) particle is 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 with V
2O
5With Li
2CO
3React the Li that makes 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 adopt the method for ion-exchange to prepare vanadium oxide water and compositions as lithium ion cathode materials as raw material.
Do not find with vanadium oxide or vanadium powder also that at present hydrogen peroxide is raw material, carbon nano-tube and organic long-chain amine are template, prepare 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 objective of the invention is take 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 take carbon nano-tube and organic long-chain amine as template in the hydro-thermal situation, get 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%.
Among the present invention, described organic long-chain amine be in lauryl amine, tetradecy lamine or the 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, form vanadium oxide colloidal sol behind the vigorous reaction; 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 is disperseed and wash to neutral;
(3) carbon nano-tube that step (2) is 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) the gluey suspension-turbid liquid of black is moved into hydrothermal reaction kettle, again reactor is placed temperature control box, through 1-10 days hydro-thermal reactions, obtain black precipitate;
(5) the gained black precipitate is carried out sintering processes under air atmosphere, obtain end product.
Among the present invention, carbon nano-tube is multi-walled carbon nano-tubes or Single Walled Carbon Nanotube described in the step (2).
Among the present invention, carbon nano-tube is disperseed in the step (2), concrete steps are: carbon nano-tube drops into the concentrated sulfuric acid and the red fuming nitric acid (RFNA) volume ratio is in the nitration mixture of 1:1-6:1, and under 30-60 ℃ of water-bath sonic oscillation 1-5 hour, then with gained carbon nano-tube water and alcohol blend washing to neutral.
Among the present invention, the organic long-chain amine described in the step (3) be in lauryl amine, tetradecy lamine or the cetylamine any.
Among the present invention, control hydrothermal reaction kettle temperature is 80-300 ℃ in the step (4).
Among the present invention, the sintering temperature under step (5) the Air atmosphere is 250-650 ℃.
Among the present invention, described vanadium oxide colloidal sol adopts the sol-gel process preparation, being about to vanadium oxide or vanadium powder mixes by mass volume ratio 1:8-1:60 (g/ml) with hydrogen peroxide (concentration is 30%), this reaction is a very exothermic and the process of emitting oxygen, just obtains subsequently orange-red vanadium oxide colloidal sol.
The present invention is take 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 characteristics.The nano-granular vanadic oxide has near the high power capacity of theoretical value and good cycle performance and large high rate performance as cathode materials for lithium battery.These good performances all have benefited from the nano-granular structure of vanadic oxide.
The nano-granular vanadic oxide that the present invention synthesized has embodied the peculiar property that the nanoscale material has aspect electrochemistry: large active surface area, can fully contact with electrolyte, and increase the active position of injecting of lithium ion, improved the capacity of electrode material; The nano-granular structure can be accelerated lithium ion transporting and effectively having alleviated in the electrochemical process lithium ion and take off the caused material volume of embedding and change therein, thereby has improved large multiplying power and the cycle performance of vanadium oxide material.
Description of drawings
Fig. 1 is the SEM(ESEM of the vanadic oxide nanoparticle for preparing of the present invention) figure.
Fig. 2 is the XRD(X x ray diffraction of the vanadic oxide nanoparticle for preparing 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 illustrates, it is important to point out that present embodiment only is used 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, with 1gV
2O
5Powder and hydrogen peroxide (30% concentration), stir at 5 ℃ of water-bath lower magnetic forces than mixing with the mass/volume of 1:10 (g/ml), will be accompanied by soon afterwards violent oxygen and heat release, about 1 hour of the whole process of putting.Generate at last orange-red vanadium oxide colloidal sol.
Two, the dispersion of carbon nano-tube
Getting original carbon nano-tube 1g adding 50mL volume ratio is in the concentrated sulfuric acid/red fuming nitric acid (RFNA) of 1:1, and sonic oscillation is 1 hour under 35 ℃ of water-baths.Went out the upper strata nitration mixture in centrifugal 10 minutes with 1000 rev/mins after the cooling, then filter, washing is to neutral.
Three, the preparation of black colloidal suspension-turbid liquid
The vanadium oxide colloidal sol of preparation and scattered 0.08g carbon nano-tube and 0.2g lauryl amine are mixed rear magnetic agitation～1 hour mutually, until the gluey suspension-turbid liquid of formation black.
Four, preparation black powder shape product under the hydrothermal condition
To carry out 2 days 100 ℃ of hydro-thermal reactions in the gluey turbid liquid immigration hydrothermal reaction kettle of black.The gained sediment is through alcohol immersion, washing and after filtering, and 100 ℃ 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 Muffle furnace, under air atmosphere, behind 350 ℃ of sintering, obtain the 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 that is 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, with 1gV
2O
3Powder and hydrogen peroxide (30% concentration), stir at 5 ℃ of water-bath lower magnetic forces than mixing with the mass/volume of 1:25 (g/ml), will be accompanied by soon afterwards violent oxygen and heat release, about 1 hour of the whole process of putting.Generate at last orange-red vanadium oxide colloidal sol.
Two, the dispersion of carbon nano-tube
Getting original carbon nano-tube 1g adding 50mL volume ratio is in the concentrated sulfuric acid/red fuming nitric acid (RFNA) of 2:1, and sonic oscillation is 2.5 hours under 40 ℃ of water-baths.Went out the upper strata nitration mixture in centrifugal 10 minutes with 1000 rev/mins after the cooling, then filter, washing is to neutral.
Three, the preparation of black colloidal suspension-turbid liquid
The vanadium oxide colloidal sol of preparation and scattered 0.12g carbon nano-tube and 0.3g lauryl amine are mixed rear magnetic agitation～1 hour mutually, until the gluey suspension-turbid liquid of formation black.
Four, preparation black powder shape product under the hydrothermal condition
To carry out 4 days 150 ℃ of hydro-thermal reactions in the gluey turbid liquid immigration hydrothermal reaction kettle of black.The gained sediment is through alcohol immersion, washing and after filtering, and 100 ℃ 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 Muffle furnace, under air atmosphere, behind 400 ℃ of sintering, obtain the 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 that is 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, with 1g vanadium powder and hydrogen peroxide (30% concentration) with the mass/volume of 1:35 (g/ml) than mixing, stir at 5 ℃ of water-bath lower magnetic forces, will be accompanied by soon afterwards violent oxygen and heat release, about 1 hour of the whole process of putting.Generate at last orange-red vanadium oxide colloidal sol.
Two, the dispersion of carbon nano-tube
Getting original carbon nano-tube 1g adding 50mL volume ratio is in the concentrated sulfuric acid/red fuming nitric acid (RFNA) of 2.5:1, and sonic oscillation is 3 hours under 45 ℃ of water-baths.Went out the upper strata nitration mixture in centrifugal 10 minutes with 1000 rev/mins after the cooling, then filter, washing is to neutral.
Three, the preparation of black colloidal suspension-turbid liquid
The vanadium oxide colloidal sol of preparation and scattered 0.15g carbon nano-tube and 0.35g lauryl amine are mixed rear magnetic agitation～1 hour mutually, until the gluey suspension-turbid liquid of formation black.
Four, preparation black powder shape product under the hydrothermal condition
To carry out 6 days 200 ℃ of hydro-thermal reactions in the gluey turbid liquid immigration hydrothermal reaction kettle of black.The gained sediment is through alcohol immersion, washing and after filtering, and 100 ℃ 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 Muffle furnace, under air atmosphere, behind 450 ℃ of sintering, obtain the 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 that is 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, with 1gVO
2Powder and hydrogen peroxide (30% concentration), stir at 5 ℃ of water-bath lower magnetic forces than mixing with the mass/volume of 1:55 (g/ml), will be accompanied by soon afterwards violent oxygen and heat release, about 1 hour of the whole process of putting.Generate at last orange-red vanadium oxide colloidal sol.
Two, the dispersion of carbon nano-tube
Getting original carbon nano-tube 1g adding 50mL volume ratio is in the concentrated sulfuric acid/red fuming nitric acid (RFNA) of 5:1, and sonic oscillation is 4 hours under 55 ℃ of water-baths.Went out the upper strata nitration mixture in centrifugal 10 minutes with 1000 rev/mins after the cooling, then filter, washing is to neutral.
Three, the preparation of black colloidal suspension-turbid liquid
The vanadium oxide colloidal sol of preparation and scattered 0.2g carbon nano-tube and 0.45g lauryl amine are mixed rear magnetic agitation～1 hour mutually, until the gluey suspension-turbid liquid of formation black.
Four, preparation black powder shape product under the hydrothermal condition
To carry out 8 days 240 ℃ of hydro-thermal reactions in the gluey turbid liquid immigration hydrothermal reaction kettle of black.The gained sediment is through alcohol immersion, washing and after filtering, and 100 ℃ 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 Muffle furnace, under air atmosphere, behind 550 ℃ of sintering, obtain the 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 that is 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.As to electrode and reference electrode, contain 1M/LLiPF with lithium metal
6Ethylene carbonate (EC) and methyl ethyl carbonate (EMC) mixed solution (Korea S Samsung 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:
Nano-granular vanadic oxide with 70% mixes with 20% carbon black, adds 10%PVDF(as binder), slowly add again 1-Methyl-2-Pyrrolidone, until Sample Dilution is also fully stirred into pasty state.Again it is applied on aluminium foil uniformly.The oven dry aluminium foil of slowly heating, first 40
oC heating 1 hour, again 80
oC heating 1 hour is at last 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.The vanadic oxide of the inventive method preparation is nano-granular as can be known, 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 surpassed 400mAh/g first, after 50 circulations, still keeps the above specific capacity of 200mAh/g; Under the high power charging-discharging (300mA/g), although capacity reduces (approximately 385mAh/g) to some extent first, after 50 circulations, the specific capacity near 200 mAh/g is arranged also.As seen, 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 characteristics.
Above-described embodiment is only in order to illustrate technological thought of the present invention and characteristics; its purpose is to make those of ordinary skill in the art can understand content of the present invention and implements according to this; the scope of this patent also not only is confined to above-mentioned specific embodiment; be all equal variation or modifications of doing according to disclosed method, still be encompassed in protection scope of the present invention.
Claims (8)
1. granular vanadic oxide cathode material for lithium ion battery of high-performance nano, it is characterized in that this battery cathode material is take carbon nano-tube and organic long-chain amine as template in the hydro-thermal situation, get 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%.
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 the cetylamine any.
3. the preparation method of 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, form vanadium oxide colloidal sol behind the vigorous reaction; 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 is disperseed and wash to neutral;
(3) carbon nano-tube that step (2) is 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) the gluey suspension-turbid liquid of black is moved into hydrothermal reaction kettle, again reactor is placed temperature control box, through 1-10 days hydro-thermal reactions, obtain black precipitate;
(5) the gained black precipitate is carried out sintering processes under air atmosphere, obtain end product.
4. preparation method according to claim 3 is characterized in that carbon nano-tube is multi-walled carbon nano-tubes or Single Walled Carbon Nanotube described in the step (2).
5. preparation method according to claim 3, it is characterized in that carbon nano-tube is disperseed in the step (2), concrete steps are: carbon nano-tube drops into the concentrated sulfuric acid and the red fuming nitric acid (RFNA) volume ratio is in the nitration mixture of 1:1-6:1, and under 30-60 ℃ of water-bath sonic oscillation 1-5 hour, then with 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 the step (3) be in lauryl amine, tetradecy lamine or the cetylamine any.
7. preparation method according to claim 3 is characterized in that control hydrothermal reaction kettle temperature is 80-300 ℃ in the step (4).
8. preparation method according to claim 2 is characterized in that the sintering temperature under step (5) the Air atmosphere is 250-650 ℃.
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| CN108899534A (en) * | 2018-06-19 | 2018-11-27 | 清华大学 | A kind of preparation method of lithium ion battery capacitor positive electrode vanadium oxide |
| 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 |
| CN115072779A (en) * | 2022-06-08 | 2022-09-20 | 攀钢集团攀枝花钢铁研究院有限公司 | Positive electrode material V of lithium ion battery 2 O 5 Nanotube and preparation method of lithium ion button battery thereof |
| 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 |
| CN115064684A (en) * | 2022-07-18 | 2022-09-16 | 陕西科技大学 | Vanadium oxide/reduced graphene oxide composite material and preparation method and application 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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