CN104600274B - Mixed polygonal vanadium oxide nanoscroll as well as preparation method and application thereof - Google Patents
Mixed polygonal vanadium oxide nanoscroll as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a mixed polygonal vanadium oxide nanoscroll as well as a preparation method thereof. The mixed polygonal vanadium oxide nanoscroll is in a multi-layer structure with open edges and a helix coil, and has a plurality of shapes, mainly triangle, quadrangle, pentagon and hexagon; the scroll is 0.5-4 microns in length; and the wall thickness of the scroll is 50-200nm. The mixed polygonal vanadium oxide nanoscroll has the beneficial effects that the polygonal nanoscroll structure is designed and constructed on the basis of a self-limited buffer mechanism; and the mixed polygonal vanadium oxide nanoscroll is successfully synthesized by a one-step hydrothermal process. The polygonal vanadium oxide nanoscroll shows excellent cycle stability and high-magnification characteristics when used as a positive electrode active material of a lithium ion battery, and is a potential application material for the lithium ion battery with high power and long service life.
Description
Technical field
The invention belongs to nano material and technical field of electrochemistry, be specifically related to a kind of mixing polygon barium oxide nanometer roll and
Preparation method, this material can be as high power extended-life lithium ion battery positive electrode active materials.
Background technology
Lithium ion battery, as a kind of Green Chemistry memory device, is widely used to mobile phone, digital camera, notebook computer etc.
Portable equipment, and progressively become the optimum selection of power mobile power supply.Although the energy density of lithium ion battery is higher, but relatively
Low lithium ion and electrons spread speed cause that its multiplying power property is poor, power density is relatively low, limit it in portable equipment
Development and the application in hybrid vehicle and pure electric automobile further；Lithium ion battery is in charge and discharge process simultaneously,
Electrode material dilation causes internal stress so that material structure destroys, and loses activity, causes cycle life to shorten, and limits
Its life-time service.And nano material have high specific surface area and preferably activity, during as lithium ion battery electrode material
, lithium ion deintercalation big with electrolyte contacts area, apart from short, can be effectively improved the electroactive of material, as high-power lithium ion electricity
During the electrode material of pond, there is significant advantage.Therefore, research Large Copacity based on novel nano electrode material, high power, longevity
Life, low cost lithium ion battery are one of forward position and focuses of current low-carbon economy epoch Study on Li-ion batteries.
As typical layered metal oxide, barium oxide nano material system is deposited because of its multiple oxidation state and coordination polyhedrom
Can reversibly embed abjection lithium ion making it have, and be considered have potential lithium ion battery material.But it is repeatedly
During embedding lithium, deterioration and the poor kinetics of crystal structure result in poor cycle performance and high rate performance.Receive
Rice roll of material there is open edge and controlled interlamellar spacing, as during lithium ion battery material in charge and discharge process available buffer swollen
Swollen shrinkage stress, prevents the structural deterioration of material, is effectively improved the cycle life of battery；And can be that ion/electronics provides
Continuous print transmission channel, improves the high rate performance of battery.In recent years, barium oxide nanometer roll material is as lithium ion cell positive
Material is progressively studied, but mixing polygon barium oxide nanometer roll electrode material is reported not yet.
Summary of the invention
The technical problem to be solved is to propose a kind of mixing polygon barium oxide nanometer roll for above-mentioned prior art
And preparation method thereof, its technique is simple, and aboundresources, the mixing polygon barium oxide nanometer roll positive electrode of gained has excellent
Good chemical property.
The present invention solves above-mentioned technical problem and be the technical scheme is that mixing polygon barium oxide nanometer roll, and it has out
The edge put, the multiple structure of helix-coil, described nanometer roll has various shape, its be mainly triangle, tetragon, five
Limit shape and hexagonal mixing, wherein roll up a length of 0.5～4 micron, and volume wall thickness is 50～200 nanometers, and it is by following method system
The standby product obtained, includes following steps:
1) 0.2mmol V is measured2O5Colloidal sol is also diluted in deionized water and obtains solution, is sufficiently stirred for；
2) in step 1) gained solution adds organic alcohol molecule, continue stirring, make solution mix homogeneously；
3) by step 2) gained solution proceeds to, in reactor, react in an oven；Take out reactor, naturally cool to room temperature；
4) by step 3) products therefrom centrifugal filtration, with deionized water and dehydrated alcohol cyclic washing gained precipitate, at baking oven
Middle drying, obtains mixing polygon barium oxide nanometer roll.
By such scheme, step 1) and step 2) described in mixing time be 1～5 hour.
By such scheme, step 2) described in organic alcohol molecule consumption be 5～6 μ L.
By such scheme, step 2) described in the unit alcohol that organic alcohol molecule is short chain or polyhydric alcohol.
By such scheme, described organic alcohol molecule be normal propyl alcohol, isopropanol, 1,2-PD, 1,3-PD, n-butyl alcohol or
N-amyl alcohol.
By such scheme, step 3) described in baking oven reaction temperature be 180～200 DEG C, the response time is 36～120 hours.
The preparation method of described mixing polygon barium oxide nanometer roll, includes following steps:
1) 0.2mmol V is measured2O5Colloidal sol is also diluted in deionized water and obtains solution, is sufficiently stirred for；
2) in step 1) gained solution adds organic alcohol molecule, continue stirring, make solution mix homogeneously；
3) by step 2) gained solution proceeds to, in reactor, react in an oven；Take out reactor, naturally cool to room temperature；
4) by step 3) products therefrom centrifugal filtration, with deionized water and dehydrated alcohol cyclic washing gained precipitate, at baking oven
Middle drying, obtains mixing polygon barium oxide nanometer roll.
Described mixing polygon barium oxide nanometer roll is as the application of anode active material of lithium ion battery.
The present invention utilizes the adjustable interlamellar spacing of mixing polygon barium oxide nanometer roll and unique polygonal shape, at material
Charge and discharge process buffer volumetric expansion stress radially and limits the interlayer slip of coil structure, thus keeping the structure of material
Integrity, improves cyclical stability and the high rate capability of material.
The invention has the beneficial effects as follows: based on certainly limiting simulated acid rain, design construction polygon nanometer roll structure, by a step
Hydro-thermal method successfully synthesizes mixing polygon barium oxide nanometer roll.When the present invention is as anode active material of lithium ion battery, should
Polygon nanometer roll show excellence cyclical stability and high-rate characteristics, be high power, extended-life lithium ion battery potential
Application material.During as anode active material of lithium ion battery, under 100mA/g electric current density, carry out constant current charge-discharge test,
Its first discharge specific capacity is up to 206mAh/g, and after circulating 150 times, specific capacity is 189mAh/g, and capability retention is 91.7%.
Under 1000mA/g high current density, its first discharge specific capacity is up to 170mAh/g, and after circulating 500 times, specific capacity is
137mAh/g, capability retention is up to 80.6%, and each capacity attenuation rate is only 0.040%.Present invention process is simple, is adopted
Simple hydro-thermal method low for equipment requirements, and the material purity prepared is high, good dispersion, it is easy to extension produces, and has very much
It is beneficial to the marketization promote.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the mixing polygon barium oxide nanometer roll of present example 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of the mixing polygon barium oxide nanometer roll of present example 1；
Fig. 3 is the transmission electron microscope picture of the mixing polygon barium oxide nanometer roll of present example 1；
Fig. 4 is the Design Mechanism figure of the mixing polygon barium oxide nanometer roll of present example 1；
Fig. 5 is the synthesis mechanism figure of the mixing polygon barium oxide nanometer roll of present example 1；
Fig. 6 is the mixing polygon barium oxide nanometer roll circulating battery under 100mA/g electric current density of present example 1
Can curve chart；
Fig. 7 is the mixing polygon barium oxide nanometer roll circulating battery under 1000mA/g electric current density of present example 1
Performance chart.
Detailed description of the invention
In order to be more fully understood that the present invention, it is further elucidated with present disclosure below in conjunction with embodiment, but present disclosure is not
It is limited only to the following examples.
Embodiment 1:
Mixing polygon barium oxide nanometer roll preparation method, it comprises the following steps:
1) 0.2mmolV is measured2O5Colloidal sol is also diluted in deionized water and obtains 60mL solution, is sufficiently stirred for；
2) in step 1) gained solution adds 5 μ L 1,2-PD organic liquids, continue stirring, make solution mix homogeneously；
3) by step 2) gained solution proceeds in 100mL reactor, reacts 36 hours under conditions of 180 DEG C；Take out anti-
Answer still, naturally cool to room temperature；
4) by step 3) products therefrom centrifugal filtration, with deionized water and dehydrated alcohol cyclic washing gained precipitate, 70
DEG C baking oven is dried, obtains mixing polygon barium oxide nanometer roll.
As it is shown in figure 5, the synthesis mechanism of the present invention is: based on hydro-thermal method, synthetic reaction process includes from crimping, oersted watt
That moral ripening, coaxial cladding crimp three processes again, have obtained mixing polygon barium oxide nanometer roll.And as shown in Figure 4,
The polygon nanometer roll structure of this uniqueness can effectively buffer electrode material charge and discharge process expanded radially shrink, limit it swollen
Interlayer slip after swollen, makes stress concentrate on edges and corners and maintains the overall structure of polygon nanometer roll, thus obtain the long-life,
Powerful chemical property.
As a example by this example product mixing polygon barium oxide nanometer roll, its structure is determined by x-ray diffractometer.Such as Fig. 1 institute
Showing, X-ray diffracting spectrum (XRD) shows, barium oxide polygon nanometer roll has good oriented growth and ordered stacks
Characteristic.As in figure 2 it is shown, field emission scanning electron microscope (FESEM) test shows, this this nanometer roll has open edge, spiral shell
The multiple structure of circumvolution song and various shape, wherein comprise triangle, tetragon, pentagon, hexagon etc., its volume a length of 0.5～4
Micron, thickness is 50～200 nanometers.As it is shown on figure 3, transmission electron microscope (TEM) and high-resolution-ration transmission electric-lens (HRTEM) test into
One step demonstrates its multiple structure.The forming process mixing polygon nanometer roll in the present invention is organic alcohol molecule absorption, Van der Waals
The result that power effect and crystal are reset.As it is shown in figure 5, the absorption of first organic alcohol molecule changes the surface tension of nano belt,
Bring it about from curling, afterwards due to the appearance of Van der Waals force and strengthen, the small molecular alcohol random distribution on nano belt surface and
Crystal is reset, and result in nano belt continuous print and bends curling at random；Then experience Ostwald ripening process is formed many
The barium oxide nanometer roll of limit shape；Then due to nanometer roll and the van der Waals interaction of nanometer interband, part nanometer roll occurs coaxial
It is coated with curly course again, finally gives mixing polygon barium oxide nanometer roll.
Mixing polygon barium oxide nanometer roll prepared by this example as anode active material of lithium ion battery, lithium ion battery
Remaining step of preparation method is identical with common preparation method.The preparation method of positive plate is as follows, uses barium oxide polygon to receive
Rice volume as active material, acetylene black as conductive agent, politef as binding agent, active material, acetylene black, poly-four
The mass ratio of fluorothene is 70:20:10；After they being sufficiently mixed in proportion, add a small amount of isopropanol, grind uniformly, right
Electrode slice thick for about 0.5mm is pressed on roller machine；The oven drying that the positive plate pressed is placed in 70 DEG C is standby after 24 hours.With 1M
LiPF6Being dissolved in vinyl carbonate (EC) and dimethyl carbonate (DMC) as electrolyte, lithium sheet is negative pole, Celgard
2325 is barrier film, and CR 2016 type rustless steel is that battery case is assembled into fastening lithium ionic cell.
The mixing polygon barium oxide nanometer roll prepared using this example is as a example by anode active material of lithium ion battery, such as Fig. 6
Shown in, under 100mA/g electric current density, carrying out constant current charge-discharge test, its first discharge specific capacity, up to 206mAh/g, is followed
After ring 150 times, specific capacity is 189mAh/g, and capability retention is 91.7%.As it is shown in fig. 7, at the big electric current of 1000mA/g
Under density, its first discharge specific capacity is up to 170mAh/g, and after circulating 500 times, specific capacity is 137mAh/g, and capacity keeps
Rate is up to 80.6%, and each capacity attenuation rate is only 0.040%.This result shows that mixing polygon barium oxide nanometer roll has excellent
Different high-rate characteristics, is the potential application material of high power, extended-life lithium ion battery.
Embodiment 2:
Mixing polygon barium oxide nanometer roll preparation method, it comprises the following steps:
1) 0.2mmol V is measured2O5Colloidal sol is also diluted in deionized water and obtains 60mL solution, is sufficiently stirred for；
2) in step 1) gained solution adds 6 μ L 1,2-PD organic liquids, continue stirring, make solution mix homogeneously；
3) by step 2) gained solution proceeds in 100mL reactor, reacts 48 hours under conditions of 180 DEG C；Take out anti-
Answer still, naturally cool to room temperature；
4) by step 3) products therefrom centrifugal filtration, with deionized water and dehydrated alcohol cyclic washing gained precipitate, 70
DEG C baking oven is dried, obtains mixing polygon barium oxide nanometer roll.
As a example by this example product, this nanometer roll has open edge, the multiple structure of helix-coil and various shape, its
In mainly contain triangle, tetragon, pentagon and hexagon, its volume a length of 0.5～4 micron, thickness is 50～200 nanometers.
The mixing polygon barium oxide nanometer roll prepared using this example is as a example by anode active material of lithium ion battery, 100
Carrying out constant current charge-discharge test under mA/g electric current density, its first discharge specific capacity is up to 206mAh/g, after circulating 150 times,
Specific capacity is 185mAh/g, and capability retention is 90.0%.
Embodiment 3:
Mixing polygon barium oxide nanometer roll preparation method, it comprises the following steps:
1) 0.2mmol V is measured2O5Colloidal sol is also diluted in deionized water and obtains 60mL solution, is sufficiently stirred for；
2) in step 1) gained solution adds 5 μ L isopropanol organic liquids, continue stirring, make solution mix homogeneously；
3) by step 2) gained solution proceeds in 100mL reactor, reacts 120 hours under conditions of 180 DEG C；Take out anti-
Answer still, naturally cool to room temperature；
4) by step 3) products therefrom centrifugal filtration, with deionized water and dehydrated alcohol cyclic washing gained precipitate, 70
DEG C baking oven is dried, obtains mixing polygon barium oxide nanometer roll.
As a example by this example product, this nanometer roll has open edge, the multiple structure of helix-coil and various shape, its
In mainly contain triangle, tetragon, pentagon and hexagon, its volume a length of 0.5～4 micron, thickness is 50～200 nanometers.
The mixing polygon barium oxide nanometer roll prepared using this example is as a example by anode active material of lithium ion battery, 100
Carrying out constant current charge-discharge test under mA/g electric current density, its first discharge specific capacity is up to 206mAh/g, after circulating 150 times,
Specific capacity is 186mAh/g, and capability retention is up to 90.3%.
Embodiment 4:
Mixing polygon barium oxide nanometer roll preparation method, it comprises the following steps:
1) 0.2mmol V is measured2O5Colloidal sol is also diluted in deionized water and obtains 60mL solution, is sufficiently stirred for；
2) in step 1) gained solution adds 5 μ L normal propyl alcohol organic liquids, continue stirring, make solution mix homogeneously；
3) by step 2) gained solution proceeds in 100mL reactor, reacts 48 hours under conditions of 180 DEG C；Take out anti-
Answer still, naturally cool to room temperature；
4) by step 3) products therefrom centrifugal filtration, with deionized water and dehydrated alcohol cyclic washing gained precipitate, 70
DEG C baking oven is dried, obtains mixing polygon barium oxide nanometer roll.
As a example by this example product, this nanometer roll has open edge, the multiple structure of helix-coil and various shape, its
In mainly contain triangle, tetragon, pentagon and hexagon, its volume a length of 0.5～4 micron, thickness is 50～200 nanometers.
The mixing polygon barium oxide nanometer roll prepared using this example is as a example by anode active material of lithium ion battery, 100
Carrying out constant current charge-discharge test under mA/g electric current density, its first discharge specific capacity is up to 204mAh/g, after circulating 150 times,
Specific capacity is 183mAh/g, and capability retention is up to 89.7%.
Embodiment 5:
Mixing polygon barium oxide nanometer roll preparation method, it comprises the following steps:
1) 0.2mmol V is measured2O5Colloidal sol is also diluted in deionized water and obtains 60mL solution, is sufficiently stirred for；
2) in step 1) gained solution adds 6 μ L n-butyl alcohol organic liquids, continue stirring, make solution mix homogeneously；
3) by step 2) gained solution proceeds in 100mL reactor, reacts 72 hours under conditions of 180 DEG C；Take out anti-
Answer still, naturally cool to room temperature；
4) by step 3) products therefrom centrifugal filtration, with deionized water and dehydrated alcohol cyclic washing gained precipitate, 70
DEG C baking oven is dried, obtains mixing polygon barium oxide nanometer roll.
As a example by this example product, this nanometer roll has open edge, the multiple structure of helix-coil and various shape, its
In mainly contain triangle, tetragon, pentagon and hexagon, its volume a length of 0.5～4 micron, thickness is 50～200 nanometers.
The mixing polygon barium oxide nanometer roll prepared using this example is as a example by anode active material of lithium ion battery, 100
Carrying out constant current charge-discharge test under mA/g electric current density, its first discharge specific capacity is up to 204mAh/g, after circulating 150 times,
Specific capacity is 182mAh/g, and capability retention is 89.2%.
Embodiment 6:
Mixing polygon barium oxide nanometer roll preparation method, it comprises the following steps:
1) 0.2mmol V is measured2O5Colloidal sol is also diluted in deionized water and obtains 60mL solution, is sufficiently stirred for；
2) in step 1) gained solution adds 6 μ L n-amyl alcohol organic liquids, continue stirring, make solution mix homogeneously；
3) by step 2) gained solution proceeds in 100mL reactor, reacts 36 hours under conditions of 200 DEG C；Take out anti-
Answer still, naturally cool to room temperature；
4) by step 3) products therefrom centrifugal filtration, with deionized water and dehydrated alcohol cyclic washing gained precipitate, 70
DEG C baking oven is dried, obtains mixing polygon barium oxide nanometer roll.
As a example by this example product, this nanometer roll has open edge, the multiple structure of helix-coil and various shape, its
In mainly contain triangle, tetragon, pentagon and hexagon, its volume a length of 0.5～4 micron, thickness is 50～200 nanometers.
The mixing polygon barium oxide nanometer roll prepared using this example is as a example by anode active material of lithium ion battery, at 100mA/g
Carrying out constant current charge-discharge test under electric current density, its first discharge specific capacity is up to 201mAh/g, after circulating 150 times, and specific capacity
For 180mAh/g, capability retention is up to 89.5%.
Claims (11)
1. mixing polygon barium oxide nanometer roll, it has open edge, the multiple structure of helix-coil, described nanometer roll
Having various shape, it is mainly triangle, tetragon, pentagon and hexagonal mixing, wherein rolls up a length of 0.5～4 micron,
Volume wall thickness is 50～200 nanometers, and it is the product prepared by following method, includes following steps:
1) 0.2mmol V is measured2O5Colloidal sol is also diluted in deionized water and obtains solution, is sufficiently stirred for；
2) in step 1) gained solution adds organic alcohol molecule, continue stirring, make solution mix homogeneously；Described Organic Alcohol
Molecule is unit alcohol or the polyhydric alcohol of short chain；
3) by step 2) gained solution proceeds to, in reactor, react in an oven；Take out reactor, naturally cool to room temperature；
4) by step 3) products therefrom centrifugal filtration, with deionized water and dehydrated alcohol cyclic washing gained precipitate, at baking oven
Middle drying, obtains mixing polygon barium oxide nanometer roll.
Mixing polygon barium oxide nanometer roll the most according to claim 1, it is characterised in that step 1) and step 2) institute
The mixing time stated is 1～5 hour.
The most according to claim 1 mixing polygon barium oxide nanometer roll, it is characterised in that step 2) described in Organic Alcohol
Molecule consumption is 5～6 μ L.
Mixing polygon barium oxide nanometer roll the most according to claim 1, it is characterised in that described organic alcohol molecule is just
Propanol, isopropanol, 1,2-propylene glycol, 1,3-propylene glycol, n-butyl alcohol or n-amyl alcohol.
The most according to claim 1 mixing polygon barium oxide nanometer roll, it is characterised in that step 3) described in baking oven anti-
Answering temperature is 180～200 DEG C, and the response time is 36～120 hours.
6. mix the preparation method of polygon barium oxide nanometer roll described in claim 1, include following steps:
1) 0.2mmol V is measured2O5Colloidal sol is also diluted in deionized water and obtains solution, is sufficiently stirred for；
2) in step 1) gained solution adds organic alcohol molecule, continue stirring, make solution mix homogeneously；Described Organic Alcohol
Molecule is unit alcohol or the polyhydric alcohol of short chain；
3) by step 2) gained solution proceeds to, in reactor, react in an oven；Take out reactor, naturally cool to room temperature；
4) by step 3) products therefrom centrifugal filtration, with deionized water and dehydrated alcohol cyclic washing gained precipitate, at baking oven
Middle drying, obtains mixing polygon barium oxide nanometer roll.
Mix the preparation method of polygon barium oxide nanometer roll the most according to claim 6, it is characterised in that step 1) and
Step 2) described in mixing time be 1～5 hour.
Mix the preparation method of polygon barium oxide nanometer roll the most according to claim 6, it is characterised in that step 2) institute
The organic alcohol molecule consumption stated is 5～6 μ L.
Mix the preparation method of polygon barium oxide nanometer roll the most according to claim 6, it is characterised in that described is organic
Alcohol molecule is normal propyl alcohol, isopropanol, 1,2-propylene glycol, 1,3-propylene glycol, n-butyl alcohol or n-amyl alcohol.
Mix the preparation method of polygon barium oxide nanometer roll the most according to claim 6, it is characterised in that step 3)
Described baking oven reaction temperature is 180～200 DEG C, and the response time is 36～120 hours.
11. mixing polygon barium oxide nanometer rolls according to claim 1 are as anode active material of lithium ion battery
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| CN103117379A (en) * | 2013-01-30 | 2013-05-22 | 武汉理工大学 | B-phase vanadium dioxide self-buffering hybrid nano-material as well as preparation method and application thereof |
| CN103553131A (en) * | 2013-10-29 | 2014-02-05 | 黑龙江大学 | Preparation method of lithium ion battery negative electrode spherical V2O3/C composite material with multilevel structure |
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| CN103553131A (en) * | 2013-10-29 | 2014-02-05 | 黑龙江大学 | Preparation method of lithium ion battery negative electrode spherical V2O3/C composite material with multilevel structure |
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