CN104176778A - Graded porous vanadium oxide microspheres and preparation method and application thereof - Google Patents
Graded porous vanadium oxide microspheres and preparation method and application thereof Download PDFInfo
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- CN104176778A CN104176778A CN201410393439.5A CN201410393439A CN104176778A CN 104176778 A CN104176778 A CN 104176778A CN 201410393439 A CN201410393439 A CN 201410393439A CN 104176778 A CN104176778 A CN 104176778A
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Abstract
The invention relates to graded porous vanadium oxide microspheres and a preparation method and application thereof. The size of the graded porous vanadium oxide microsphere is 4-10 micrometers, and the graded porous vanadium oxide microspheres are structurally formed by stacking a plurality of nano particles in a staggered way. The preparation method of the graded porous vanadium oxide microspheres comprises the following steps of: dissolving ammonium metavanadate in an organic solvent, carrying out condensation refluxing for 1-4 hours at constant temperature of 150-190 DEG C so that ammonium metavanadate has a reduction reaction to obtain bluish violet vanadium alkoxide precipitate; placing the bluish violet vanadium alkoxide precipitate in an argon atmosphere and calcining at 200-700 DEG C for 3-6 hours to obtain the graded porous vanadium oxide microspheres. According to the preparation method, the graded porous vanadium oxide microspheres are prepared by adopting constant-temperature liquid-phase reaction, related raw materials are common and nontoxic, the used process is simple and easy to operate, and high output is achieved; and the obtained graded porous vanadium oxide microsphere has important application value in the field of electrodes of lithium ion batteries.
Description
Technical field
The invention belongs to inorganic materials and electrochemical device technical field, be specifically related to a kind of classifying porous barium oxide microballoon and preparation method thereof, this material can be used as the material at lithium ion or other electrochemical devices.
Background technology
Along with the aggravation consumption of the irreversible energy such as oil, portable energy source system faces increasingly serious challenge.Lithium ion battery, because its higher energy density, good cycle performance and stronger retention of charge are considered to be expected to replace oil, is widely used in portable electron device.But the positive electrode material that at present commercialization and being about to enters explorative research is embedding lithium transition-metal oxide mostly, these positive electrode materials exist that fatal intrinsic restriction---lower specific storage, is difficult to realize fast charging and discharging.Therefore need development of new positive electrode material to meet high-energy-density, powerful requirement.Wherein, barium oxide is because have higher capacity, reserves are abundant, relative low price, this makes barium oxide have good application prospect as cell positive material, likely meet requirement and hybrid vehicle (HV) and electromobile (EV) requirement to high-energy-density and high power battery of portable electron device to high-quality battery, become one of positive electrode material of new generation of current primary study.
At present, every research mainly improves its storage lithium performance by surface properties, internal structure, size and the pattern of regulation and control barium oxide.Barium oxide, comprises V
2o
5, VO
2, V
2o
3the structure such as nano wire, nanometer rod, nanotube and nano particle there is report or the patent of being correlated with.The people such as professor Huang Wanxia of Sichuan University utilize CTAB to do template, adopt the method for hydro-thermal to synthesize vanadium dioxide nano sheet, and be made into electrode test storage lithium performance [Na Li, Wanxia Wang, Qiwu Shi, Yubo Zhang, Linwei Song, Ceramics International, 2013,39,6199-6206].Above-mentioned report adopts hydrothermal method mostly, react temperature required height, time length, yield poorly, and the barium oxide preparing belongs to nano-scale, in height removal lithium embedded process, there is serious volume effect, there is particle agglomeration, cause the cyclical stability of electrode to decline, in actual production, be unfavorable for large-scale application.
Therefore, further regulate and control size, pattern and the internal structure of barium oxide, and improve its preparation technology and condition, there is very important application value.
Summary of the invention
The object of the present invention is to provide a kind of classifying porous barium oxide microballoon and its preparation method and application, it is more common that the method desired raw material is reported before, preparation method is simple, and classifying porous barium oxide microballoon is applied to and prepares lithium ion cell electrode and show excellent chemical property.
For achieving the above object, the technical solution used in the present invention is:
A kind of classifying porous barium oxide microballoon, microballoon size 4～10 μ m, described micro-sphere structure is to be formed by the interlaced accumulation of multiple porous nano particles.
According to technique scheme, described barium oxide is undefined structure, and described nanoparticle is that length is the triangular prism shape of 200-300nm; Or described barium oxide is vanadium dioxide, described nanoparticle is that length is the porous triangular prism shape of 300～500nm; Or described barium oxide is vanadous oxide, described nanoparticle is particulate state.
A preparation method for classifying porous barium oxide microballoon, comprises the following steps:
(1) take 0.2～0.6g ammonium meta-vanadate, add 100～400mL organic solvent, 40～80 DEG C of magnetic agitation in water-bath, the glassy yellow precursor liquid of formation homogeneous transparent;
(2) precursor liquid step (1) being obtained continues to be placed in 150～190 DEG C of reaction 1～4h of thermostatical oil bath, and in reaction process, at unlimited system condensing reflux, ammonium meta-vanadate is reduced, and obtains bluish voilet precipitation;
(3) precipitation that step (2) obtained is centrifugal, clean and dry;
(4) by the powder transfer of drying in step (3) in tube furnace, in argon gas atmosphere, temperature is to calcine 3～6h under the condition of 200～700 DEG C, obtains classifying porous barium oxide microballoon.
According to technique scheme, described organic solvent is to adopt ethylene glycol, Diethylene Glycol and Macrogol 200 one wherein.
According to technique scheme, the preferred heat-up rate of described calcination process is 1 DEG C/min, and preferred calcination temperature is 200～700 DEG C, and preferably calcination time is 3～6h.
The classifying porous barium oxide microballoon of preparing according to such scheme, is applied to lithium ion cell positive, shows good chemical property.
Compared with prior art, the invention has the beneficial effects as follows:
(1) materials safety, the cheapness, pollution-free that the present invention relates to, the ammonium meta-vanadate of use and organic solvent are common drug, do not use poisonous and hazardous organic surface active agent and additive.
(2) the simple environmental protection of technique of the present invention, to reaction vessel, there is no particular limitation, reaction safety and stability, repeatability is high, and output is very large, meets the requirement of production application.
(3) temperature that the present invention can calcine by adjusting regulates and controls the crystal formation of barium oxide, prepares the barium oxide of multiple crystal formation.
(4) the porous barium oxide microballoon that prepared by the present invention has hierarchical porous structure, be applied to and prepare lithium ion cell positive, many active surfaces can provide more embedding lithium/de-lithium avtive spot relatively, shortened Li+ ion diffusion length, improved charge transport efficiency, and, can also effectively alleviate the volume change of active material while discharging and recharging, thereby the cyclical stability of strongthener, improve the chemical property of lithium ion battery, met the demand to high energy storage device in actual production.
Brief description of the drawings
Fig. 1 is the XRD figure of the porous barium oxide microballoon that makes in the embodiment of the present invention 1.
Fig. 2 is the SEM figure of the porous barium oxide microballoon that makes in the embodiment of the present invention 1.
Fig. 3 is the XRD figure of the porous barium oxide microballoon that makes in the embodiment of the present invention 2.
Fig. 4 is the SEM figure of the porous barium oxide microballoon that makes in the embodiment of the present invention 2.
Fig. 5 is the TEM figure of the porous barium oxide microballoon that makes in the embodiment of the present invention 2.
Fig. 6 is the XRD figure of the porous barium oxide microballoon that makes in the embodiment of the present invention 3.
Fig. 7 is the SEM figure of the porous barium oxide microballoon that makes in the embodiment of the present invention 3.
Fig. 8 is the XRD figure of the porous barium oxide microballoon that makes in the embodiment of the present invention 4.
Fig. 9 is the SEM figure of the porous barium oxide microballoon that makes in the embodiment of the present invention 4.
Figure 10 is the XRD figure of the porous barium oxide microballoon that makes in the embodiment of the present invention 5.
Figure 11 is the SEM figure of the porous barium oxide microballoon that makes in the embodiment of the present invention 5.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
Embodiment 1:
A synthetic method for porous barium oxide microballoon, comprises following steps:
(1) 0.5g ammonium meta-vanadate is joined in 200mL ethylene glycol, be placed in 80 DEG C of stirring 1h on water-bath, form the glassy yellow liquid of homogeneous transparent;
(2) mixing solutions step (1) Suo Shu is continued to be placed on oil bath pan, be warming up to 170 DEG C, then at 170 DEG C of isothermal reaction 2h, condensing reflux in reaction process, then naturally cooling, obtains bluish voilet precipitation;
(3) precipitation step (2) being obtained is placed on whizzer and cleans six times with ethanol, and centrifuge speed is 6000r/min, then the centrifugal powder obtaining is dried in 60 DEG C of baking ovens;
(4) powder of step (3) being dried is placed in tube furnace, from room temperature, is warmed up to 300 DEG C with the speed of 1 DEG C/min, and 300 DEG C of insulations 5 hours, obtains porous barium oxide microballoon.
The product that the present embodiment obtains is defined as unformed porous barium oxide microballoon through X-ray diffraction analysis, and its X-ray diffractogram is shown in Fig. 1.The demonstration of scanning electron microscope analysis result, the microballoon that this product is porous, is of a size of 7 microns of left and right, and the existence form in hole is for piling up hole, and its SEM figure is shown in Fig. 2.Be applied to lithium ion cell electrode, can improve the chemical property of lithium ion battery.
The unformed porous barium oxide microballoon that the present embodiment is made is made into the positive pole of lithium ion battery, show good chemical property: the result of button half-cell test shows, under the current density of 50mA/g, the first circle specific discharge capacity of battery reaches 148mAh/g, after discharging and recharging 50 circles, reversible specific capacity still has 65mAh/g.
Embodiment 2:
A synthetic method for porous barium oxide microballoon, comprises following steps:
(1) 0.5g ammonium meta-vanadate is joined in 400mL ethylene glycol, be placed in 60 DEG C of stirring 30min on water-bath, form the glassy yellow liquid of homogeneous transparent;
(2) mixing solutions step (1) Suo Shu is continued to be placed on oil bath pan, be warming up to 170 DEG C, then at 170 DEG C of isothermal reaction 1h, condensing reflux in reaction process, then naturally cooling, obtains bluish voilet precipitation;
(3) precipitation step (2) being obtained is placed on whizzer and cleans six times with ethanol, and centrifuge speed is 6000r/min, then the centrifugal powder obtaining is dried in 60 DEG C of baking ovens;
(4) powder of step (3) being dried is placed in tube furnace, from room temperature, is warmed up to 500 DEG C with the speed of 1 DEG C/min, and 500 DEG C of insulations 4 hours, obtains porous barium oxide microballoon.
The product that the present embodiment obtains is defined as vanadium dioxide crystal through X-ray diffraction analysis, and its X-ray diffractogram is shown in Fig. 3.The demonstration of scanning electron microscope analysis result, this product is classifying porous micron ball, is of a size of 6 microns of left and right, and the length of porous triangular prism is about 450nm, and its SEM figure is shown in Fig. 4.Transmission electron microscope the results are shown in Figure 5, result shows that the vanadium dioxide microballoon obtaining has hierarchical porous structure, is applied to lithium ion cell electrode, and more embedding lithium/de-lithium avtive spot can be provided, shorten the transmission route of lithium ion, improve the chemical property of lithium ion battery.
The classifying porous vanadium dioxide microballoon that the present embodiment is made is made into the positive pole of lithium ion battery, show good chemical property: the result of button half-cell test shows, under the current density of 50mA/g, the first circle specific discharge capacity of battery is up to 250mAh/g, after discharging and recharging 50 circles, reversible specific capacity still has 140mAh/g.
Embodiment 3:
A synthetic method for porous barium oxide microballoon, comprises following steps:
(1) 0.25g ammonium meta-vanadate is joined in 200mL ethylene glycol, be placed in 80 DEG C of stirring 2h on water-bath, form the glassy yellow liquid of homogeneous transparent;
(2) mixing solutions step (1) Suo Shu is continued to be placed on oil bath pan, be warming up to 180 DEG C, then at 180 DEG C of isothermal reaction 2h, condensing reflux in reaction process, then naturally cooling, obtains bluish voilet precipitation;
(3) precipitation step (2) being obtained is placed on whizzer and cleans six times with ethanol, and centrifuge speed is 6000r/min, then the centrifugal powder obtaining is dried in 60 DEG C of baking ovens;
(4) powder of step (3) being dried is placed in tube furnace, from room temperature, is warmed up to 600 DEG C with the speed of 1 DEG C/min, and 600 DEG C of insulations 5 hours, obtains porous barium oxide microballoon.
The product that the present embodiment obtains is defined as the mixed phase of vanadium dioxide and vanadous oxide through X-ray diffraction analysis, its X-ray diffractogram is shown in Fig. 6.Scanning electronic microscope result shows, the microballoon that this product is porous, and microballoon is about by length that the triangular prism subsiding of 500nm form, and microballoon is of a size of about 5 μ m, and its SEM figure is shown in Fig. 7.The barium oxide microballoon that the present embodiment is made is made into the positive pole of lithium ion battery, show good chemical property: the result of button half-cell test shows, under the current density of 50mA/g, the first circle specific discharge capacity of battery is about 190mAh/g, after discharging and recharging 50 circles, reversible specific capacity still has 130mAh/g.
Embodiment 4:
A synthetic method for porous barium oxide microballoon, comprises following steps:
(1) 1g ammonium meta-vanadate is joined in 200mL ethylene glycol, be placed in 40 DEG C of stirring 1h on water-bath, form the glassy yellow liquid of homogeneous transparent;
(2) mixing solutions step (1) Suo Shu is continued to be placed on oil bath pan, be warming up to 170 DEG C, then at 170 DEG C of isothermal reaction 2h, condensing reflux in reaction process, then naturally cooling, obtains bluish voilet precipitation;
(3) precipitation step (2) being obtained is placed on whizzer and cleans six times with ethanol, and centrifuge speed is 6000r/min, then the centrifugal powder obtaining is dried in 60 DEG C of baking ovens;
(4) powder of step (3) being dried is placed in tube furnace, from room temperature, is warmed up to 700 DEG C with the speed of 1 DEG C/min, and 700 DEG C of insulations 5 hours, obtains porous barium oxide microballoon.
The product that the present embodiment obtains is defined as vanadous oxide crystal through X-ray diffraction analysis, and its X-ray diffractogram is shown in Fig. 8.The demonstration of scanning electronic microscope result, this product is the microballoon of the porous of shape homogeneous, is of a size of 7 μ m left and right, and the nanometer small-particle that surface is 20-150nm by length is piled up and is formed, and its SEM figure is shown in Fig. 9.
The barium oxide microballoon that the present embodiment is made is made into the positive pole of lithium ion battery, show good chemical property: the result of button half-cell test shows, under the current density of 50mA/g, the first circle specific discharge capacity of battery reaches 190mAh/g, after discharging and recharging 50 circles, reversible specific capacity still has 120mAh/g.
Embodiment 5:
A synthetic method for porous barium oxide microballoon, comprises following steps:
(1) 1g ammonium meta-vanadate is joined in 200mL Diethylene Glycol, be placed in 40 DEG C of stirring 1h on water-bath, form the glassy yellow liquid of homogeneous transparent;
(2) mixing solutions step (1) Suo Shu is continued to be placed on oil bath pan, be warming up to 150 DEG C, then at 150 DEG C of isothermal reaction 2h, condensing reflux in reaction process, then naturally cooling, obtains bluish voilet precipitation;
(3) precipitation step (2) being obtained is placed on whizzer and cleans six times with ethanol, and centrifuge speed is 6000r/min, then the centrifugal powder obtaining is dried in 60 DEG C of baking ovens;
(4) powder of step (3) being dried is placed in tube furnace, from room temperature, is warmed up to 600 DEG C with the speed of 1 DEG C/min, and 600 DEG C of insulations 3 hours, obtains porous barium oxide microballoon.
The product that the present embodiment obtains is defined as barium oxide mixed phase crystal through X-ray diffraction analysis, and its X-ray diffractogram is shown in Figure 10.Scanning electronic microscope result shows, the microballoon that this product is porous, and this microballoon form for the nanometer rod of 40nm is staggered by being about, and microballoon is of a size of about 6 μ m, wherein has the fragmentation of part ball, and its SEM figure is shown in Figure 11.
The barium oxide microballoon that the present embodiment is made is made into the positive pole of lithium ion battery, the chemical property showing: the result of button half-cell test shows, under the current density of 50mA/g, the first circle specific discharge capacity of battery reaches 200mAh/g, after discharging and recharging 50 circles, reversible specific capacity still has 100mAh/g.
The cited each raw material of the present invention can be realized the present invention, and the bound value of each raw material, interval value can realize the present invention, bound value and the interval value of processing parameter of the present invention (as temperature, time etc.) can be realized the present invention, do not enumerate embodiment at this.
Claims (6)
1. a classifying porous barium oxide microballoon, is characterized in that, described microballoon is of a size of 4～10 μ m, and described micro-sphere structure is to be formed by the interlaced accumulation of multiple nanoparticles.
2. classifying porous barium oxide microballoon according to claim 1, is characterized in that, described barium oxide is undefined structure, and described nanoparticle is that length is the triangular prism shape of 200-300nm; Or described barium oxide is vanadium dioxide, described nanoparticle is that length is the porous triangular prism shape of 300～500nm; Or described barium oxide is vanadous oxide, described nanoparticle is particulate state.
3. a preparation method for classifying porous barium oxide microballoon, comprises the following steps:
(1) take 0.2～0.6g ammonium meta-vanadate, add 100～400mL organic solvent, 40～80 DEG C of magnetic agitation in water-bath, the glassy yellow precursor liquid of formation homogeneous transparent;
(2) precursor liquid step (1) being obtained continues to be placed in 150～190 DEG C of reaction 1～4h of constant temperature oil bath, in reaction process, at unlimited system condensing reflux, obtains bluish voilet precipitation;
(3) precipitation that step (2) obtained is centrifugal, clean and dry;
(4) by the powder transfer of drying in step (3) in tube furnace, in argon gas atmosphere, temperature is to calcine 3～6h under the condition of 200～700 DEG C, obtains classifying porous barium oxide microballoon.
4. the preparation method of a kind of classifying porous barium oxide microballoon according to claim 3, is characterized in that, described organic solvent is the one in ethylene glycol, Diethylene Glycol and Macrogol 200.
5. the preparation method of a kind of classifying porous barium oxide microballoon according to claim 3, is characterized in that, the heat-up rate of described calcination process is 1 DEG C/min, and calcining temperature is 200～700 DEG C, and calcination time is 3～6h.
6. classifying porous barium oxide microballoon according to claim 1 is as the application of anode active material of lithium ion battery.
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| CN105118977A (en) * | 2015-09-02 | 2015-12-02 | 武汉理工大学 | V2O5 hollow micron wire ball with nano wire three-dimensional winding structure and preparation method and application thereof |
| CN105236487A (en) * | 2015-10-20 | 2016-01-13 | 辽宁石油化工大学 | Vanadium oxide nanosphere and preparation method thereof |
| CN106006733A (en) * | 2016-05-16 | 2016-10-12 | 武汉理工大学 | Method for preparing vanadium trioxide through hydrothermal method |
| CN106006736A (en) * | 2016-05-16 | 2016-10-12 | 武汉理工大学 | Method of using hydrogen for preparing vanadium trioxide from vanadium-containing solution |
| CN109133171A (en) * | 2018-11-09 | 2019-01-04 | 吉林大学 | A kind of spherical porous pattern VO of different-diameter size2And preparation method thereof |
| CN109368694A (en) * | 2018-11-09 | 2019-02-22 | 吉林大学 | The spherical porous R phase V of different-diameter size2O3And preparation method thereof |
| CN110021746A (en) * | 2019-04-24 | 2019-07-16 | 青海民族大学 | A kind of preparation method and lithium ion battery of carbon coating vanadium trioxide |
| CN111584247A (en) * | 2020-05-20 | 2020-08-25 | 璧靛悍 | V-shaped groove2O5Nitrogen-sulfur-loaded double-doped porous carbon supercapacitor electrode material and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105118977A (en) * | 2015-09-02 | 2015-12-02 | 武汉理工大学 | V2O5 hollow micron wire ball with nano wire three-dimensional winding structure and preparation method and application thereof |
| CN105236487A (en) * | 2015-10-20 | 2016-01-13 | 辽宁石油化工大学 | Vanadium oxide nanosphere and preparation method thereof |
| CN106006733A (en) * | 2016-05-16 | 2016-10-12 | 武汉理工大学 | Method for preparing vanadium trioxide through hydrothermal method |
| CN106006736A (en) * | 2016-05-16 | 2016-10-12 | 武汉理工大学 | Method of using hydrogen for preparing vanadium trioxide from vanadium-containing solution |
| CN109133171A (en) * | 2018-11-09 | 2019-01-04 | 吉林大学 | A kind of spherical porous pattern VO of different-diameter size2And preparation method thereof |
| CN109368694A (en) * | 2018-11-09 | 2019-02-22 | 吉林大学 | The spherical porous R phase V of different-diameter size2O3And preparation method thereof |
| CN110021746A (en) * | 2019-04-24 | 2019-07-16 | 青海民族大学 | A kind of preparation method and lithium ion battery of carbon coating vanadium trioxide |
| CN111584247A (en) * | 2020-05-20 | 2020-08-25 | 璧靛悍 | V-shaped groove2O5Nitrogen-sulfur-loaded double-doped porous carbon supercapacitor electrode material and preparation method thereof |
| CN111584247B (en) * | 2020-05-20 | 2021-11-05 | 重庆普朗电气设备有限公司 | V-shaped groove2O5Nitrogen-sulfur-loaded double-doped porous carbon supercapacitor electrode material and preparation method thereof |
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