CN102683665B - Lithium-vanadium oxide over-long nano wire and preparation method and application thereof - Google Patents
Lithium-vanadium oxide over-long nano wire and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a lithium-vanadium oxide over-long nano wire and a preparation method thereof. The lithium-vanadium oxide over-long nano wire can be taken as an anode active material for a high-power long-service-life lithium ion battery, is 200-300 microns in length, and is 100-200 nanometers in diameter. The lithium-vanadium oxide over-long nano wire is obtained in a simple calcining way. When the lithium-vanadium oxide over-long nano wire is taken as an anode active material for the lithium ion battery, the discharge capacity can still be up to 120mAh/g after circulating at the current density of 2,000mA/g for 600 times, and the capacity attenuation ratio per time is only 0.022 percent. As proved by a result, the lithium-vanadium oxide over-long nano wire has excellent high magnification characteristic, and is a potential application material for the high-power long-service-life lithium ion battery. In a simple hydro-thermal method adopted for preparing a precursor H2V3O8 over-long nano wire, the shape and size of a material can be controlled by changing the reactant concentration, reaction temperature and time, and the prepared material has high purity and high dispersivity.
Description
Technical field
The invention belongs to nano material and technical field of electrochemistry, be specifically related to a kind of lithium-barium oxide overlong nanowire and preparation method thereof, it can be used as high power extended-life lithium ion battery positive electrode active materials.
Background technology
Lithium ion battery, as a kind of green energy resource, has been widely used in the portable equipment such as mobile phone, notebook computer.Although the energy density of lithium ion battery is higher, lower lithium ion and electrons spread speed cause that its multiplying power property is poor, power density is lower.Multiplying power property is poor is that the required charging interval of battery is longer, and this limits further developing in its portable equipment; Lower power density has limited the application of lithium ion battery in hybrid vehicle and pure electric automobile.Therefore, large capacity, high power, long-life, the low cost lithium ion battery of research based on novel nano electrode material is one of the forward position of current low-carbon economy epoch Study on Li-ion batteries using and focus.Nano-material has large draw ratio, high specific area and electronics confinement effect radially and axial electron transport property, during as lithium ion battery electrode material and electrolyte contact area is large, lithium ion deintercalation distance is short, can effectively improve the electroactive of material, during as high power lithium ion cell electrode material, there is significant advantage.
As typical layered metal oxide, barium oxide nano material system enjoys attention because the existence of its multiple oxidation state and coordination polyhedrom makes it have the open architecture that can embed metal ion, and is regarded as potential lithium ion battery material and has obtained long-range development.Lithium-barium oxide is in keeping barium oxide layer structure, and the lithium ion of its interlayer is by ionic bond and upper and lower V
3o
8layer interacts and makes it in cyclic process, keep stable structure.In recent years, although lithium-barium oxide is widely studied as anode material for lithium-ion batteries, have compared with rarely seen report of the lithium-barium oxide nano wire of high length-diameter ratio.
Summary of the invention
The object of the present invention is to provide a kind of lithium-barium oxide overlong nanowire, it has good electric chemical property.
Another object of the present invention is to provide the preparation method of the simple lithium-barium oxide overlong nanowire of a kind of technique.
The present invention solves the problems of the technologies described above adopted technical scheme: lithium-barium oxide overlong nanowire, and its length reaches 200 ~ 300 microns, and diameter is 100 ~ 200 nanometers, adopts following method to make, and includes following steps:
1) get V
2o
5powder is put into ceramic crucible and is placed in Muffle furnace, heats and is incubated to molten condition;
2) by step 1) gained melting V
2o
5pour rapidly quenching in deionized water at normal temperature into, gained heating liquid to boiling is not stopped to stir, cooling rear suction filtration, obtains V by filtrate leaving standstill
2o
5colloidal sol, demarcates its concentration, for subsequent use;
3) measure step 2) V of gained 1.1 ~ 1.5 mmol
2o
5colloidal sol is also diluted in and in deionized water, obtains 40 mL V
2o
5solution, presses and V
2o
5amount of substance splashes into V than the aniline solution that measures 0.05 mol/L for 0.03:1
2o
5solution, stirs 0.5 hour;
4) take PEG-4000 0.02 ~ 0.06 g and be dissolved in 15 mL deionized waters, this solution is added in step 3) gained solution and adds deionized water to overall solution volume is 60 mL;
5) step 4) gained solution is continued to stirring one day at room temperature ageing one day, then proceed in 100 mL reactors, react, then from reactor, take out, naturally cool to room temperature;
6) product centrifugal filtration step 5) being obtained, with deionized water cyclic washing gained sediment, obtains H after being dried
2v
3o
8overlong nanowire;
7) take step 6) gained 0.1 g H
2v
3o
8nano wire is scattered in 10 mL absolute ethyl alcohols, and the lithium source that takes respective amount adds above-mentioned solution, stirs 5 hours, then mixture is dried to obtain to hybrid solid in 80 ℃ of air dry ovens;
8) dried step 7) gained hybrid solid is transferred to ceramic crucible and is placed in Muffle furnace sintering, finally obtain product lithium-barium oxide overlong nanowire.
The technical scheme that the preparation method of lithium-barium oxide overlong nanowire adopts is to include following steps:
1) get V
2o
5powder is put into ceramic crucible and is placed in Muffle furnace, heats and is incubated to molten condition;
2) by step 1) gained melting V
2o
5pour rapidly quenching in deionized water at normal temperature into, gained heating liquid to boiling is not stopped to stir, cooling rear suction filtration, obtains V by filtrate leaving standstill
2o
5colloidal sol, demarcates its concentration, for subsequent use;
3) measure step 2) V of gained 1.1 ~ 1.5 mmol
2o
5colloidal sol is also diluted in and in deionized water, obtains 40 mL V
2o
5solution, presses and V
2o
5amount of substance splashes into V than the aniline solution that measures 0.05 mol/L for 0.03:1
2o
5solution, stirs 0.5 hour;
4) take PEG-4000 0.02 ~ 0.06 g and be dissolved in 15 mL deionized waters, this solution is added in step 3) gained solution and adds deionized water to overall solution volume is 60 mL;
5) step 4) gained solution is continued to stirring one day at room temperature ageing one day, then proceed in 100 mL reactors, react, then from reactor, take out, naturally cool to room temperature;
6) product centrifugal filtration step 5) being obtained, with deionized water cyclic washing gained sediment, obtains H after being dried
2v
3o
8overlong nanowire;
7) take step 6) gained 0.1 g H
2v
3o
8nano wire is scattered in 10 mL absolute ethyl alcohols, and the lithium source that takes respective amount adds above-mentioned solution, stirs 5 hours, then mixture is dried to obtain to hybrid solid in 80 ℃ of air dry ovens;
8) dried step 7) gained hybrid solid is transferred to ceramic crucible and is placed in Muffle furnace sintering, finally obtain product lithium-barium oxide overlong nanowire.
Press such scheme, the reaction temperature described in step 5) is 160 ~ 200 ℃; The described reaction time is 36 ~ 60 hours;
Press such scheme, described lithium source is lithium hydroxide, lithium carbonate or lithium acetate, and wherein lithium/vanadium mol ratio is 1.05 ~ 1.25:3.
Press such scheme, the sintering temperature described in step 8) is 400 ~ 500 ℃; Described sintering time is 5 ~ 15 hours.
Lithium-barium oxide overlong nanowire is in the application aspect anode active material of lithium ion battery.
The invention has the beneficial effects as follows: selection of the present invention and lithium-barium oxide have the H of similar layer structure
2v
3o
8overlong nanowire, as presoma, by simple calcining, obtains lithium-barium oxide overlong nanowire.During as anode active material of lithium ion battery, under the current density of 2000 mA/g, the discharge capacity after 600 times that circulates still can reach 120 mAh/g, and each capacity attenuation rate is only 0.022 %.This result shows that lithium-barium oxide overlong nanowire has excellent high magnification characteristic, is the potential application material of high power, extended-life lithium ion battery.
In addition, prepare presoma H
2v
3o
8the simple hydro thermal method that overlong nanowire adopts, can control by changing reactant concentration, reaction temperature and time pattern and the size of material, and the material purity making is high, good dispersion.And it is simple, low for equipment requirements to prepare the simple calcination method technique that lithium-barium oxide overlong nanowire adopts, is very beneficial for the marketization and promotes.
Accompanying drawing explanation
Fig. 1 is the lithium-barium oxide Li of embodiment 1
(1+x)v
3o
8(x=0) XRD of overlong nanowire figure;
Fig. 2 is the lithium-barium oxide Li of embodiment 1
(1+x)v
3o
8(x=0) the low multiplication factor FESEM figure of overlong nanowire;
Fig. 3 is the lithium-barium oxide Li of embodiment 1
(1+x)v
3o
8(x=0) overlong nanowire and presoma H
2v
3o
8the FESEM figure of nano wire; Wherein, Fig. 3 (a) is presoma H
2v
3o
8the FESEM figure of nano wire, Fig. 3 (b) is Li
(1+x)v
3o
8(x=0) FESEM of overlong nanowire figure;
Fig. 4 is the lithium-barium oxide Li of embodiment 1
(1+x)v
3o
8(x=0) TEM of overlong nanowire figure;
Fig. 5 is the lithium-barium oxide Li of embodiment 1
(1+x)v
3o
8(x=0) the cycle performance of battery curve chart of overlong nanowire.
Embodiment
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1:
Lithium-barium oxide Li
(1+x)v
3o
8(x=0) preparation method of overlong nanowire, it comprises the steps:
1) take 20 g V
2o
5powder is put into ceramic crucible and is placed in Muffle furnace, is warming up to 800 ℃, is incubated and within 0.5 hour, makes its abundant melting;
2) by melting V
2o
5pour rapidly quenching in 2 L deionized water at normal temperature into, the rufous liquid obtaining is heated to boiling on electric furnace and does not stop to stir 1 hour, cooling rear suction filtration is removed residual solids three times, and filtrate leaving standstill obtained to stable peony V for seven days
2o
5colloidal sol, gets three parts, 10 mL colloidal sol sample, takes respectively quality and calculate collosol concentration after oven dry, averages and is V
2o
5collosol concentration, for subsequent use;
3) measure the V of 1.3 mmol
2o
5colloidal sol is also diluted in and in deionized water, obtains 40 mL solution, by and V
2o
5amount of substance splashes into V than the aniline solution that measures 0.05 mol/L for 0.03:1
2o
5solution, stirs 0.5 hour;
4) take PEG-4000 0.04 g and be dissolved in 15 mL deionized waters, this solution is added to upper step 3) gained solution and adds deionized water to overall solution volume is 60 mL;
5) gained solution is continued to stirring one day at room temperature ageing one day, then proceed in 100 mL reactors, under 180 ℃ of conditions, react 48 hours, take out reactor, naturally cool to room temperature;
6) by the product centrifugal filtration obtaining, with deionized water cyclic washing gained sediment, in 80 ℃ of baking ovens, dry, obtain H
2v
3o
8(also referred to as V
3o
7h
2o) overlong nanowire;
7) take 0.1 g H
2v
3o
8nano wire is scattered in 10 mL absolute ethyl alcohols, and the lithium hydroxide that takes respective amount take lithium/vanadium mol ratio as the ratio of 1.05:3 adds above-mentioned solution, stirs 5 hours, then mixture is dried in 80 ℃ of air dry ovens;
8) dried hybrid solid is transferred to ceramic crucible and is placed in Muffle furnace, sintering 10 hours at 450 ℃, finally obtains lithium-barium oxide overlong nanowire (product).
Take the embodiment of the present invention 1 products therefrom lithium-barium oxide overlong nanowire as example, its structure is determined by x-ray diffractometer.As shown in Figure 1, lithium-barium oxide overlong nanowire is LiV substantially
3o
8phase (JCPDS card number is 01-072-1193), containing micro-dephasign is Li
0.3v
2o
5.As shown in Figure 2, lithium-barium oxide overlong nanowire has kept presoma H substantially
2v
3o
8the pattern of nano wire, length can reach 300 microns, and Fig. 3 shows that the diameter of nano wire is 100 ~ 200 nanometers.Fig. 4 is transmission electron microscope (TEM) and selected area electron diffraction (SAED) test result, show that this nano wire has obvious mono-crystalline structures, and the direction of growth is <001> direction.
Lithium-barium oxide overlong nanowire prepared by the present invention is as anode active material of lithium ion battery, and all the other steps of the preparation method of lithium ion battery are identical with common preparation method.The preparation method of positive plate is as follows, adopts lithium-barium oxide overlong nanowire as active material, and acetylene black is as conductive agent, and polytetrafluoroethylene is as binding agent, and the mass ratio of active material, acetylene black, polytetrafluoroethylene is 70:20:10; After they are fully mixed in proportion, add a small amount of isopropyl alcohol, grind evenly, on twin rollers, press the thick electrode slice of approximately 0.5 mm; It is for subsequent use after 24 hours that the positive plate pressing is placed in the oven drying of 80 ℃.With the LiPF of 1 M
6be dissolved in vinyl carbonate (EC) and dimethyl carbonate (DMC) as electrolyte, lithium sheet is negative pole, and Celgard 2325 is barrier film, and CR 2025 type stainless steels are that battery case is assembled into fastening lithium ionic cell.
As shown in Figure 5, take lithium-barium oxide overlong nanowire as example, under the current density of 1500 mA/g, this nano wire can reach 160 mAh/g in the discharge capacity after 400 times that circulates, and each capacity attenuation rate is only 0.025 %.Under the current density of 2000 mA/g, the discharge capacity after 600 times that circulates still reaches 120 mAh/g, and each capacity attenuation rate is only 0.022 %.This result shows that lithium-barium oxide overlong nanowire has excellent high magnification characteristic, is the potential application material of high power, extended-life lithium ion battery.
Embodiment 2:
Lithium-barium oxide Li
(1+x)v
3o
8(x=0.1) preparation method of overlong nanowire, it comprises the steps:
1) take 20 g V
2o
5powder is put into ceramic crucible and is placed in Muffle furnace, is warming up to 800 ℃, is incubated and within 0.5 hour, makes its abundant melting;
2) by melting V
2o
5pour rapidly quenching in 2 L deionized water at normal temperature into, the rufous liquid obtaining is heated to boiling on electric furnace and does not stop to stir 1 hour, cooling rear suction filtration is removed residual solids three times, and filtrate leaving standstill obtained to stable peony V for seven days
2o
5colloidal sol, gets three parts, 10 mL colloidal sol sample, takes respectively quality and calculate collosol concentration after oven dry, averages and is V
2o
5collosol concentration, for subsequent use;
3) measure the V of 1.5 mmol
2o
5colloidal sol is also diluted in and in deionized water, obtains 40 mL solution, by and V
2o
5amount of substance splashes into V than the aniline solution that measures 0.05 mol/L for 0.03:1
2o
5solution, stirs 0.5 hour;
4) take PEG-4000 0.06 g and be dissolved in 15 mL deionized waters, this solution is added to upper step 3) gained solution and adds deionized water to overall solution volume is 60 mL;
5) gained solution is continued to stirring one day at room temperature ageing one day, then proceed in 100 mL reactors, under 180 ℃ of conditions, react 48 hours, take out reactor, naturally cool to room temperature;
6) by the product centrifugal filtration obtaining, with deionized water cyclic washing gained sediment, in 80 ℃ of baking ovens, dry, obtain H
2v
3o
8(also referred to as V
3o
7h
2o) overlong nanowire;
7) take 0.1 g H
2v
3o
8nano wire is scattered in 10 mL absolute ethyl alcohols, and the lithium carbonate that takes respective amount take lithium/vanadium mol ratio as the ratio of 1.15:3 adds above-mentioned solution, stirs 5 hours, then mixture is dried in 80 ℃ of air dry ovens;
8) dried hybrid solid is transferred to ceramic crucible and is placed in Muffle furnace, at 450 ℃, sintering 5 hours, finally obtains lithium-barium oxide Li
(1+x)v
3o
8(x=0.1) overlong nanowire (product).
This example gained lithium-barium oxide overlong nanowire length can reach approximately 250 microns, and diameter is 100 ~ 200 nanometers.Under the current density of 1500 mA/g, this nano wire is 147 mAh/g in the discharge capacity after 400 times that circulates, and each capacity attenuation rate is 0.032 %.Under the current density of 2000 mA/g, the discharge capacity after 600 times that circulates is 112 mAh/g, and each capacity attenuation rate is 0.027 %.
Embodiment 3:
Lithium-barium oxide Li
(1+x)v
3o
8(x=0.2) preparation method of overlong nanowire, it comprises the steps:
1) take 20 g V
2o
5powder is put into ceramic crucible and is placed in Muffle furnace, is warming up to 800 ℃, is incubated and within 0.5 hour, makes its abundant melting;
2) by melting V
2o
5pour rapidly quenching in 2 L deionized water at normal temperature into, the rufous liquid obtaining is heated to boiling on electric furnace and does not stop to stir 1 hour, cooling rear suction filtration is removed residual solids three times, and filtrate leaving standstill obtained to stable peony V for seven days
2o
5colloidal sol, gets three parts, 10 mL colloidal sol sample, takes respectively quality and calculate collosol concentration after oven dry, averages and is V
2o
5collosol concentration, for subsequent use;
3) measure the V of 1.1 mmol
2o
5colloidal sol is also diluted in and in deionized water, obtains 40 mL solution, by and V
2o
5amount of substance splashes into V than the aniline solution that measures 0.05 mol/L for 0.03:1
2o
5solution, stirs 0.5 hour;
4) take PEG-4000 0.02 g and be dissolved in 15 mL deionized waters, this solution is added to upper step 3) gained solution and adds deionized water to overall solution volume is 60 mL;
5) gained solution is continued to stirring one day at room temperature ageing one day, then proceed in 100 mL reactors, under 200 ℃ of conditions, react 36 hours, take out reactor, naturally cool to room temperature;
6) by the product centrifugal filtration obtaining, with deionized water cyclic washing gained sediment, in 80 ℃ of baking ovens, dry, obtain H
2v
3o
8(also referred to as V
3o
7h
2o) overlong nanowire;
7) take 0.1 g H
2v
3o
8nano wire is scattered in 10 mL absolute ethyl alcohols, and the lithium acetate that takes respective amount take lithium/vanadium mol ratio as the ratio of 1.25:3 adds above-mentioned solution, stirs 5 hours, then mixture is dried in 80 ℃ of air dry ovens;
8) dried hybrid solid is transferred to ceramic crucible and is placed in Muffle furnace, at 400 ℃, sintering 15 hours, finally obtains Li
(1+x)v
3o
8(x=0.2) overlong nanowire (product).
This example gained lithium-barium oxide overlong nanowire length can reach approximately 280 microns, and diameter is 150 ~ 200 nanometers.Under the current density of 1500 mA/g, this nano wire is 151 mAh/g in the discharge capacity after 400 times that circulates, and each capacity attenuation rate is 0.030 %.Under the current density of 2000 mA/g, the discharge capacity after 600 times that circulates is 114 mAh/g, and each capacity attenuation rate is 0.025 %.
Embodiment 4:
Lithium-barium oxide Li
(1+x)v
3o
8(x=0) preparation method of overlong nanowire, it comprises the steps:
1) take 20 g V
2o
5powder is put into ceramic crucible and is placed in Muffle furnace, is warming up to 800 ℃, is incubated and within 0.5 hour, makes its abundant melting;
2) by melting V
2o
5pour rapidly quenching in 2 L deionized water at normal temperature into, the rufous liquid obtaining is heated to boiling on electric furnace and does not stop to stir 1 hour, cooling rear suction filtration is removed residual solids three times, and filtrate leaving standstill obtained to stable peony V for seven days
2o
5colloidal sol, gets three parts, 10 mL colloidal sol sample, takes respectively quality and calculate collosol concentration after oven dry, averages and is V
2o
5collosol concentration, for subsequent use;
3) measure the V of 1.3 mmol
2o
5colloidal sol is also diluted in and in deionized water, obtains 40 mL solution, by and V
2o
5amount of substance splashes into V than the aniline solution that measures 0.05 mol/L for 0.03:1
2o
5solution, stirs 0.5 hour;
4) take PEG-4000 0.04 g and be dissolved in 15 mL deionized waters, this solution is added to upper step 3) gained solution and adds deionized water to overall solution volume is 60 mL;
5) gained solution is continued to stirring one day at room temperature ageing one day, then proceed in 100 mL reactors, under 160 ℃ of conditions, react 60 hours, take out reactor, naturally cool to room temperature;
6) by the product centrifugal filtration obtaining, with deionized water cyclic washing gained sediment, in 80 ℃ of baking ovens, dry, obtain H
2v
3o
8(also referred to as V
3o
7h
2o) overlong nanowire;
7) take 0.1 g H
2v
3o
8nano wire is scattered in 10 mL absolute ethyl alcohols, and the lithium hydroxide that takes respective amount take lithium/vanadium mol ratio as the ratio of 1.05:3 adds above-mentioned solution, stirs 5 hours, then mixture is dried in 80 ℃ of air dry ovens;
8) dried hybrid solid is transferred to ceramic crucible and is placed in Muffle furnace, at 500 ℃, sintering 5 hours, finally obtains Li
(1+x)v
3o
8(x=0) overlong nanowire (product).
This example gained lithium-barium oxide overlong nanowire length can reach approximately 300 microns, and diameter is 100 ~ 200 nanometers.Under the current density of 1500 mA/g, this nano wire is 155 mAh/g in the discharge capacity after 400 times that circulates, and each capacity attenuation rate is 0.027 %.Under the current density of 2000 mA/g, the discharge capacity after 600 times that circulates is 116 mAh/g, and each capacity attenuation rate is 0.023 %.
Embodiment 5:
Lithium-barium oxide Li
(1+x)v
3o
8(x=0.2) preparation method of overlong nanowire, it comprises the steps:
1) take 20 g V
2o
5powder is put into ceramic crucible and is placed in Muffle furnace, is warming up to 800 ℃, is incubated and within 0.5 hour, makes its abundant melting;
2) by melting V
2o
5pour rapidly quenching in 2 L deionized water at normal temperature into, the rufous liquid obtaining is heated to boiling on electric furnace and does not stop to stir 1 hour, cooling rear suction filtration is removed residual solids three times, and filtrate leaving standstill obtained to stable peony V for seven days
2o
5colloidal sol, gets three parts, 10 mL colloidal sol sample, takes respectively quality and calculate collosol concentration after oven dry, averages and is V
2o
5collosol concentration, for subsequent use;
3) measure the V of 1.3 mmol
2o
5colloidal sol is also diluted in and in deionized water, obtains 40 mL solution, by and V
2o
5amount of substance splashes into V than the aniline solution that measures 0.05 mol/L for 0.03:1
2o
5solution, stirs 0.5 hour;
4) take PEG-4000 0.04 g and be dissolved in 15 mL deionized waters, this solution is added to upper step 3) gained solution and adds deionized water to overall solution volume is 60 mL;
5) gained solution is continued to stirring one day at room temperature ageing one day, then proceed in 100 mL reactors, under 180 ℃ of conditions, react 48 hours, take out reactor, naturally cool to room temperature;
6) by the product centrifugal filtration obtaining, with deionized water cyclic washing gained sediment, in 80 ℃ of baking ovens, dry, obtain H
2v
3o
8(also referred to as V
3o
7h
2o) overlong nanowire;
7) take 0.1 g H
2v
3o
8nano wire is scattered in 10 mL absolute ethyl alcohols, and the lithium hydroxide that takes respective amount take lithium/vanadium mol ratio as the ratio of 1.25:3 adds above-mentioned solution, stirs 5 hours, then mixture is dried in 80 ℃ of air dry ovens;
8) dried hybrid solid is transferred to ceramic crucible and is placed in Muffle furnace, at 400 ℃, sintering 15 hours, finally obtains Li
(1+x)v
3o
8(x=0.2) overlong nanowire (product).
This example gained lithium-barium oxide overlong nanowire length can reach approximately 300 microns, and diameter is 100 ~ 200 nanometers.Under the current density of 1500 mA/g, this nano wire is 135 mAh/g in the discharge capacity after 400 times that circulates, and each capacity attenuation rate is 0.038 %.Under the current density of 2000 mA/g, the discharge capacity after 600 times that circulates is 108 mAh/g, and each capacity attenuation rate is 0.033 %.
Claims (9)
1. lithium-barium oxide overlong nanowire, its chemical formula is Li
(1+x)v
3o
8, wherein 0≤x≤0.2, its length reaches 200 ~ 300 microns, and diameter is 100 ~ 200 nanometers, adopts following method to make, and includes following steps:
1) get V
2o
5powder is put into ceramic crucible and is placed in Muffle furnace, heats and is incubated to molten condition;
2) by step 1) gained melting V
2o
5pour rapidly quenching in deionized water at normal temperature into, gained heating liquid to boiling is not stopped to stir, cooling rear suction filtration, obtains V by filtrate leaving standstill
2o
5colloidal sol, demarcates its concentration, for subsequent use;
3) measure step 2) V of gained 1.1 ~ 1.5 mmol
2o
5colloidal sol is also diluted in and in deionized water, obtains 40 mL V
2o
5solution, by aniline and V
2o
5amount of substance splashes into V than the aniline solution that measures 0.05 mol/L for 0.03:1
2o
5solution, stirs 0.5 hour;
4) take PEG-4000 0.02 ~ 0.06 g and be dissolved in 15 mL deionized waters, this solution is added in step 3) gained solution and adds deionized water to overall solution volume is 60 mL;
5) step 4) gained solution is continued to stirring one day at room temperature ageing one day, then proceed in 100 mL reactors, react, then from reactor, take out, naturally cool to room temperature;
6) product centrifugal filtration step 5) being obtained, with deionized water cyclic washing gained sediment, obtains H after being dried
2v
3o
8overlong nanowire;
7) take step 6) gained 0.1 g H
2v
3o
8nano wire is scattered in 10 mL absolute ethyl alcohols, and the lithium source that takes respective amount adds above-mentioned solution, stirs 5 hours, then mixture is dried to obtain to hybrid solid in 80 ℃ of air dry ovens;
8) dried step 7) gained hybrid solid is transferred to ceramic crucible and is placed in Muffle furnace sintering, finally obtain product lithium-barium oxide overlong nanowire.
2. lithium-barium oxide overlong nanowire as claimed in claim 1, is characterized in that the reaction temperature described in step 5) is 160 ~ 200 ℃; The described reaction time is 36 ~ 60 hours.
3. lithium-barium oxide overlong nanowire as claimed in claim 1, is characterized in that described lithium source is lithium hydroxide, lithium carbonate or lithium acetate, and wherein lithium/vanadium mol ratio is 1.05 ~ 1.25:3.
4. lithium-barium oxide overlong nanowire as claimed in claim 1, is characterized in that the sintering temperature described in step 8) is 400 ~ 500 ℃; Described sintering time is 5 ~ 15 hours.
5. the preparation method of lithium-barium oxide overlong nanowire claimed in claim 1, is characterized in that including following steps:
1) get V
2o
5powder is put into ceramic crucible and is placed in Muffle furnace, heats and is incubated to molten condition;
2) by step 1) gained melting V
2o
5pour rapidly quenching in deionized water at normal temperature into, gained heating liquid to boiling is not stopped to stir, cooling rear suction filtration, obtains V by filtrate leaving standstill
2o
5colloidal sol, demarcates its concentration, for subsequent use;
3) measure step 2) V of gained 1.1 ~ 1.5 mmol
2o
5colloidal sol is also diluted in and in deionized water, obtains 40 mL V
2o
5solution, by aniline and V
2o
5amount of substance splashes into V than the aniline solution that measures 0.05 mol/L for 0.03:1
2o
5solution, stirs 0.5 hour;
4) take PEG-4000 0.02 ~ 0.06 g and be dissolved in 15 mL deionized waters, this solution is added in step 3) gained solution and adds deionized water to overall solution volume is 60 mL;
5) step 4) gained solution is continued to stirring one day at room temperature ageing one day, then proceed in 100 mL reactors, react, then from reactor, take out, naturally cool to room temperature;
6) product centrifugal filtration step 5) being obtained, with deionized water cyclic washing gained sediment, obtains H after being dried
2v
3o
8overlong nanowire;
7) take step 6) gained 0.1 g H
2v
3o
8nano wire is scattered in 10 mL absolute ethyl alcohols, and the lithium source that takes respective amount adds above-mentioned solution, stirs 5 hours, then mixture is dried to obtain to hybrid solid in 80 ℃ of air dry ovens;
8) dried step 7) gained hybrid solid is transferred to ceramic crucible and is placed in Muffle furnace sintering, finally obtain product lithium-barium oxide overlong nanowire.
6. the preparation method of lithium-barium oxide overlong nanowire as claimed in claim 5, is characterized in that the reaction temperature described in step 5) is 160 ~ 200 ℃; The described reaction time is 36 ~ 60 hours.
7. the preparation method of lithium-barium oxide overlong nanowire as claimed in claim 5, is characterized in that, described lithium source is lithium hydroxide, lithium carbonate or lithium acetate, and wherein lithium/vanadium mol ratio is 1.05 ~ 1.25:3.
8. the preparation method of lithium-barium oxide overlong nanowire as claimed in claim 5, is characterized in that the sintering temperature described in step 8) is 400 ~ 500 ℃; Described sintering time is 5 ~ 15 hours.
9. lithium-barium oxide overlong nanowire claimed in claim 1 is in the application aspect anode active material of lithium ion battery.
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