CN104176778B - A kind of classifying porous barium oxide microballoon and its preparation method and application - Google Patents
A kind of classifying porous barium oxide microballoon and its preparation method and application Download PDFInfo
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- CN104176778B CN104176778B CN201410393439.5A CN201410393439A CN104176778B CN 104176778 B CN104176778 B CN 104176778B CN 201410393439 A CN201410393439 A CN 201410393439A CN 104176778 B CN104176778 B CN 104176778B
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Abstract
The present invention relates to a kind of classifying porous barium oxide microballoon and its preparation method and application, wherein, microballoon is of a size of 4 ~ 10 μm, and described micro-sphere structure is formed by the interlaced accumulation of multiple nanoparticle.The preparation method of described microballoon comprises: dissolved in organic solvent by ammonium meta-vanadate, and be placed in 150 ~ 190 DEG C of constant-temperature condensation backflow 1 ~ 4h, ammonium meta-vanadate generation reduction reaction obtains the alkoxide bluish voilet precipitation of vanadium, this precipitation is placed in argon gas atmosphere, at 200 ~ 700 DEG C of calcining 3 ~ 6h, obtain classifying porous barium oxide microballoon.The present invention adopts constant temperature liquid phase reaction to prepare classifying porous barium oxide microballoon, and the raw material related to is common nontoxic, simple for process, and output is comparatively large, and the porous barium oxide microballoon obtained has important using value in lithium ion cell electrode field.
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, excellent cycle performance and stronger retention of charge, is considered to be expected to replace oil, is widely used in portable electron device.But the positive electrode material that current 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, rich reserves, relative low price, this makes barium oxide have good application prospect as cell positive material, likely meet portable electron device to the requirement to high-energy-density and high power battery of the requirement of high-quality battery and hybrid vehicle (HV) and electromobile (EV), one of positive electrode material of new generation becoming current primary study.
At present, every research improves its storage lithium performance mainly through regulating and controlling the surface properties of barium oxide, internal structure, size and pattern.Barium oxide, comprises V
2o
5, VO
2, V
2o
3nano wire, nanometer rod, the structure such as nanotube and nano particle there is the report of being correlated with or patent.The people such as professor Huang Wanxia of Sichuan University utilize CTAB to do template, the method of hydro-thermal is adopted to synthesize vanadium dioxide nano sheet, and be made into electrode test storage lithium performance [NaLi, WanxiaWang, QiwuShi, YuboZhang, LinweiSong, CeramicsInternational, 2013,39,6199-6206].Above-mentioned report adopts hydrothermal method mostly, react temperature required height, time length, yield poorly, and the barium oxide prepared 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, regulate and control the size of barium oxide, pattern and internal structure further, 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 comparatively 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, Microsphere Size 4 ~ 10 μm, described micro-sphere structure is formed by the interlaced accumulation of multiple porous nano particles.
According to technique scheme, described barium oxide is undefined structure, the triangular prism shape of described nanoparticle to be length be 200-300nm; Or described barium oxide is vanadium dioxide, the porous triangular prism shape of described nanoparticle to be length be 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, form the glassy yellow precursor liquid of homogeneous transparent;
(2) continued by the precursor liquid that step (1) obtains to be placed in thermostatical oil bath 150 ~ 190 DEG C reaction 1 ~ 4h, at unlimited system condensing reflux in reaction process, ammonium meta-vanadate is reduced, and obtains bluish voilet precipitation;
(3) pelleting centrifugation step (2) obtained, cleaning drying;
(4) by the powder transfer of drying in step (3) in tube furnace, in argon gas atmosphere, temperature is calcine 3 ~ 6h under the condition of 200 ~ 700 DEG C, obtains classifying porous barium oxide microballoon.
According to technique scheme, described organic solvent adopts 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 preferred calcination time is 3 ~ 6h.
According to classifying porous barium oxide microballoon prepared by such scheme, be applied to lithium ion cell positive, show good chemical property.
Compared with prior art, the invention has the beneficial effects as follows:
(1) materials safety that the present invention relates to, cheapness, pollution-free, 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 present invention process, to reaction vessel, there is no particular limitation, reaction safety and stability, and repeatability is high, and output is very large, meets the requirement of production application.
(3) the present invention by the crystal formation regulating the temperature of calcining to regulate and control barium oxide, can prepare 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, relatively many active surfaces can provide more embedding lithium/de-lithium avtive spot, shorten the diffusion length of Li+ ion, improve charge transport efficiency, and, effectively can also alleviate the volume change of active material during discharge and recharge, thus the cyclical stability of strongthener, improve the chemical property of lithium ion battery, meet the demand to high energy storage device in actual production.
Accompanying drawing explanation
Fig. 1 is the XRD figure of porous barium oxide microballoon obtained in the embodiment of the present invention 1.
Fig. 2 is the SEM figure of porous barium oxide microballoon obtained in the embodiment of the present invention 1.
Fig. 3 is the XRD figure of porous barium oxide microballoon obtained in the embodiment of the present invention 2.
Fig. 4 is the SEM figure of porous barium oxide microballoon obtained in the embodiment of the present invention 2.
Fig. 5 is the TEM figure of porous barium oxide microballoon obtained in the embodiment of the present invention 2.
Fig. 6 is the XRD figure of porous barium oxide microballoon obtained in the embodiment of the present invention 3.
Fig. 7 is the SEM figure of porous barium oxide microballoon obtained in the embodiment of the present invention 3.
Fig. 8 is the XRD figure of porous barium oxide microballoon obtained in the embodiment of the present invention 4.
Fig. 9 is the SEM figure of porous barium oxide microballoon obtained in the embodiment of the present invention 4.
Figure 10 is the XRD figure of porous barium oxide microballoon obtained in the embodiment of the present invention 5.
Figure 11 is the SEM figure of porous barium oxide microballoon obtained in the embodiment of the present invention 5.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, 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, be 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) continued to be placed on oil bath pan by the mixing solutions described in step (1), be warming up to 170 DEG C, then at 170 DEG C of isothermal reaction 2h, condensing reflux in reaction process, then naturally cooling, obtain bluish voilet precipitation;
(3) precipitation that step (2) obtains be placed on whizzer and use ethanol purge six times, centrifuge speed is 6000r/min, is then dried in 60 DEG C of baking ovens by the centrifugal powder obtained;
(4) powder that step (3) is 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, obtain 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.Scanning electron microscope analysis result shows, and this product is the microballoon of porous, is of a size of 7 microns, 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, the chemical property of lithium ion battery can be improved.
The unformed porous barium oxide microballoon obtained by the present embodiment is made into the positive pole of lithium ion battery, show good chemical property: the result display of button half-cell test, under the current density of 50mA/g, the first circle specific discharge capacity of battery reaches 148mAh/g, after discharge and recharge 50 is enclosed, 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) continued to be placed on oil bath pan by the mixing solutions described in step (1), be warming up to 170 DEG C, then at 170 DEG C of isothermal reaction 1h, condensing reflux in reaction process, then naturally cooling, obtain bluish voilet precipitation;
(3) precipitation that step (2) obtains be placed on whizzer and use ethanol purge six times, centrifuge speed is 6000r/min, is then dried in 60 DEG C of baking ovens by the centrifugal powder obtained;
(4) powder that step (3) is 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, obtain 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.Scanning electron microscope analysis result shows, and this product is classifying porous micron ball, is of a size of 6 microns, 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 obtained has hierarchical porous structure, is applied to lithium ion cell electrode, can provide more embedding lithium/de-lithium avtive spot, shorten the transmission route of lithium ion, improve the chemical property of lithium ion battery.
The classifying porous vanadium dioxide microballoon obtained by the present embodiment is made into the positive pole of lithium ion battery, show good chemical property: the result display of button half-cell test, under the current density of 50mA/g, the first circle specific discharge capacity of battery is up to 250mAh/g, after discharge and recharge 50 is enclosed, 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) continued to be placed on oil bath pan by the mixing solutions described in step (1), be warming up to 180 DEG C, then at 180 DEG C of isothermal reaction 2h, condensing reflux in reaction process, then naturally cooling, obtain bluish voilet precipitation;
(3) precipitation that step (2) obtains be placed on whizzer and use ethanol purge six times, centrifuge speed is 6000r/min, is then dried in 60 DEG C of baking ovens by the centrifugal powder obtained;
(4) powder that step (3) is 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, obtain 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, and its X-ray diffractogram is shown in Fig. 6.Scanning electronic microscope result shows, and this product is the microballoon of porous, and microballoon is about by length that the triangular prism subsided of 500nm forms, and microballoon is of a size of about 5 μm, and its SEM figure is shown in Fig. 7.The barium oxide microballoon obtained by the present embodiment is made into the positive pole of lithium ion battery, show good chemical property: the result display of button half-cell test, under the current density of 50mA/g, the first circle specific discharge capacity of battery is about 190mAh/g, after discharge and recharge 50 is enclosed, 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) continued to be placed on oil bath pan by the mixing solutions described in step (1), be warming up to 170 DEG C, then at 170 DEG C of isothermal reaction 2h, condensing reflux in reaction process, then naturally cooling, obtain bluish voilet precipitation;
(3) precipitation that step (2) obtains be placed on whizzer and use ethanol purge six times, centrifuge speed is 6000r/min, is then dried in 60 DEG C of baking ovens by the centrifugal powder obtained;
(4) powder that step (3) is 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, obtain 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.Scanning electronic microscope result shows, and this product is the microballoon of the homogeneous porous of shape, is of a size of about 7 μm, and the nanometer small-particle that surface is 20-150nm by length is piled up and formed, and its SEM figure is shown in Fig. 9.
The barium oxide microballoon obtained by the present embodiment is made into the positive pole of lithium ion battery, show good chemical property: the result display of button half-cell test, under the current density of 50mA/g, the first circle specific discharge capacity of battery reaches 190mAh/g, after discharge and recharge 50 is enclosed, 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) continued to be placed on oil bath pan by the mixing solutions described in step (1), be warming up to 150 DEG C, then at 150 DEG C of isothermal reaction 2h, condensing reflux in reaction process, then naturally cooling, obtain bluish voilet precipitation;
(3) precipitation that step (2) obtains be placed on whizzer and use ethanol purge six times, centrifuge speed is 6000r/min, is then dried in 60 DEG C of baking ovens by the centrifugal powder obtained;
(4) powder that step (3) is 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, obtain 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, and this product is the microballoon of porous, and this microballoon is by being about as the nanometer rod of 40nm is interlocked and form, and microballoon is of a size of about 6 μm, wherein has part ball broken, and its SEM figure is shown in Figure 11.
The barium oxide microballoon obtained by the present embodiment is made into the positive pole of lithium ion battery, the chemical property shown: the result display of button half-cell test, under the current density of 50mA/g, the first circle specific discharge capacity of battery reaches 200mAh/g, after discharge and recharge 50 is enclosed, reversible specific capacity still has 100mAh/g.
Each raw material cited by the present invention can realize 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 realize the present invention, do not enumerate embodiment at this.
Claims (5)
1. a classifying porous barium oxide microballoon, it is characterized in that, described Microsphere Size is 4 ~ 10 μm, and described micro-sphere structure is formed by the interlaced accumulation of multiple nanoparticle, described barium oxide is undefined structure, the triangular prism shape of described nanoparticle to be length be 200-300nm; Or described barium oxide is vanadium dioxide, the porous triangular prism shape of described nanoparticle to be length be 300 ~ 500nm; Or described barium oxide is vanadous oxide, described nanoparticle is particulate state.
2. the preparation method of a kind of classifying porous barium oxide microballoon according to claim 1, 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, form the glassy yellow precursor liquid of homogeneous transparent;
(2) precursor liquid that step (1) obtains is continued be placed in constant temperature oil bath 150 ~ 190 DEG C reaction 1 ~ 4h, at unlimited system condensing reflux in reaction process, obtain bluish voilet precipitation;
(3) pelleting centrifugation step (2) obtained, cleaning drying;
(4) by the powder transfer of drying in step (3) in tube furnace, in argon gas atmosphere, temperature is calcine 3 ~ 6h under the condition of 200 ~ 700 DEG C, obtains classifying porous barium oxide microballoon.
3. the preparation method of a kind of classifying porous barium oxide microballoon according to claim 2, it is characterized in that, described organic solvent is the one in ethylene glycol, Diethylene Glycol and Macrogol 200.
4. the preparation method of a kind of classifying porous barium oxide microballoon according to claim 2, 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.
5. 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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| CN105236487B (en) * | 2015-10-20 | 2017-07-18 | 辽宁石油化工大学 | A kind of barium oxide nanosphere and preparation method thereof |
| CN106006736B (en) * | 2016-05-16 | 2017-06-13 | 武汉理工大学 | Using hydrogen from the method containing vanadium trioxide is prepared in vanadium solution |
| CN106006733B (en) * | 2016-05-16 | 2017-06-13 | 武汉理工大学 | A kind of method that hydro-thermal method prepares vanadium trioxide |
| 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 |
| CN109133171B (en) * | 2018-11-09 | 2020-09-22 | 吉林大学 | VO with spherical porous morphology and different diameter sizes2And method for preparing the same |
| 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 |
| 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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