CN109437302A - It is a kind of to prepare the spherical porous pattern V of different-diameter size2O5Method - Google Patents
It is a kind of to prepare the spherical porous pattern V of different-diameter size2O5Method Download PDFInfo
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- CN109437302A CN109437302A CN201811328715.4A CN201811328715A CN109437302A CN 109437302 A CN109437302 A CN 109437302A CN 201811328715 A CN201811328715 A CN 201811328715A CN 109437302 A CN109437302 A CN 109437302A
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Abstract
It is of the invention a kind of to prepare the spherical porous pattern V of different-diameter size2O5Method, belong to the technical field of micro-nano functional material preparation.The first step of preparation method is mixed using ammonium metavanadate, hydroxylamine hydrochloride with ethylene glycol as raw material, and mixed solution prepares the precursor VEG of different-diameter size by different mixings time with hydro-thermal method；Second step will be calcined 3~4 hours at precursor VEG in air 300~600 DEG C, prepare spherical, porous V2O5Pattern.Calcining has the advantages that easy to operate, Portable safety, low-temperature energy-saving, reproducible in the hydrothermal synthesis and air that the present invention has；Only it can be obtained by different-diameter size product by controlling mixed solution mixing time；The spherical porous V of the high-purity of product, different-diameter size2O5New pattern is good anode material in lithium ion battery.
Description
Technical field
The invention belongs to the technical fields of micro-nano functional material preparation.
Background technique
Nanotechnology is the scientific research and production of the broad covered area, multi-crossed disciplines that grow up the 1990s
Industry field, particularly in recent years, the energy lacks more and more prominent with problem of environmental pollution, and the fast development of nanotechnology is
It solves energy and environment crisis and provides endless possibility, so the preparation method of some micro Nano materials with excellent characteristics
It is explored by scientific research personnel always.
And a kind of resource of the barium oxide as rich content, have a variety of oxidation states, its excellent properties make its
It is widely applied in the fields such as catalysis, battery, magnetics and absorption.The oxide of vanadium also has their unique physics and chemistry
Characteristic, to have a wide range of applications, for example, being used as the electrode material of catalyst, chemical sensor, high density lithium battery, together
When some barium oxides be also widely used in various optics, in electronic equipment.
The research of recent barium oxide micro Nano material receives the widely concern of people, barium oxide micro Nano material
Microstructure such as dimension, size, pattern have a great impact for performances such as the light of device, electricity, magnetic, catalysis.And use letter
It is single that industrialized synthetic method is convenient for prepare the micro Nano material that particle is tiny, of uniform size, pattern is uniform, dispersion degree is high,
It is the premise for preparing high performance material device.Have much about the method for preparing barium oxide nano material, such as hydro-thermal at present
(solvent heat) method, sol-gel method, oxidation-reduction method etc., but need to find a kind of system for preparing vanadic anhydride of simplicity
Preparation Method.
V2O5Pattern mainly have nano wire V2O5, nano-powder V2O5, nanocrystal V2O5, nano thin-film V2O5And it synthesizes
V2O5The method of different-shape also has very much, mainly there is sol-gel method, hydro-thermal method etc..
But utilize spherical, the porous V of hydro-thermal method synthesis different-diameter size2O5It has not been reported.
Spherical, the porous V of preparation2O5New pattern can be used as anode material in lithium ion battery, this is mainly due to
V2O5Not only there are no pollution to the environment for positive electrode as lithium battery, but also its unique three-dimensional structure.Electrolyte can be improved
With the contact area of barium oxide, and lithium ion diffusion length is effectively shortened, therefore spherical, porous V2O5New pattern can be
Anode material is used as in lithium ion battery.
Method of the invention is using ammonium metavanadate, hydroxylamine hydrochloride and ethylene glycol as raw material, at (160 DEG C of lower hydrothermal temperature
~170 DEG C) and the shorter time (can be 10~15 hours) under, different-diameter ruler can be prepared by different mixings time
Very little precursor VEG (vanadic acid ethylene glycol rouge), the diameter dimension of precursor VEG within a certain period of time can be with mixed solution mixing time
Increase and increase, but the diameter dimension of precursor VEG will not increase with the increase of the time of heating, the diameter of precursor VEG
Size is distributed between 1~11 μm.Then by under different calcination conditions to the spherical of prepared different-diameter size
Micro-nano spherical, the porous V of different-diameter size can be obtained in precursor VEG calcining2O5New pattern.
Summary of the invention
The technical problem to be solved by the present invention is to prepared the precursor of different-diameter size by hydro-thermal method, then led to
It crosses calcining and has prepared different-diameter size spherical shape, porous V2O5New pattern
Method provided by the invention is, prepares spherical vanadic acid ethylene glycol rouge (VEG) precursor using hydro-thermal method, then by
Calcined precursors VEG (vanadic acid ethylene glycol rouge) obtains spherical, porous V in air2O5New pattern.And hair is probed by a series of
The spherical diameter size of existing precursor VEG is related with the mixing time of mixed solution, is specifically controlling the constant feelings of other variables
Under condition, precursor VEG spherical diameter size can increase with the increase of mixed solution mixing time.It may then pass through to difference
The precursor VEG calcining of diameter dimension can prepare the spherical porous V of different-diameter size2O5New pattern, obtained spherical shape are more
The V in hole2O5It has been effectively maintained the pattern of precursor vanadic acid ethylene glycol rouge (VEG) spherical shape.
The specific technical solution of the present invention is as follows.
It is a kind of to prepare the spherical porous pattern V of different-diameter size2O5Method, prepare precursor vanadic acid ethylene glycol rouge
(VEG), the V of spherical porous pattern is prepared2O5Process；
The process for preparing precursor vanadic acid ethylene glycol rouge is that hydrochloric acid hydroxyl is added after mixing ammonium metavanadate and ethylene glycol
Amine obtains mixed solution, wherein the molar ratio of ammonium metavanadate and hydroxylamine hydrochloride is 2:3~3.1, ammonium metavanadate and ethylene glycol
Molar ratio is 1:715~718；Mixed solution is transferred to reaction kettle after 1000~1500 revs/min are stirred 0.5~8 hour
In polytetrafluoroethyllining lining, reacted 10~35 hours under the conditions of 160~170 DEG C；Separation of solid and liquid obtains purple red precipitate, centrifugation
Washing, frozen drying obtain precursor vanadic acid ethylene glycol rouge (VEG)；
The V for preparing spherical porous pattern2O5Process, be by precursor vanadic acid ethylene glycol rouge (VEG) in air
It is calcined 3~4 hours at 300~600 DEG C, prepares spherical, porous V2O5Pattern.
When ammonium metavanadate and hydroxylamine hydrochloride are mixed in ethylene glycol, precursor VEG spherical diameter size is in a timing
It is interior to increase with the increase of mixed solution mixing time.It can then be obtained by calcining the precursor VEG of different-diameter size
Obtain spherical, the porous V essentially identical with precursor diameter dimension2O5New pattern.
The ethylene glycol, the density selected are 1.111~1.115g/ml.
Described is transferred in reaction kettle polytetrafluoroethyllining lining, and packing ratio is (that is, mixed solution accounts for reaction kettle polytetrafluoroethyl-ne
The ratio of alkene liner volume) it is 80%.
The centrifuge washing is to purple red precipitate deionized water and dehydrated alcohol centrifuge washing 5 times；Described is low
Temperature freeze-drying, is by the precipitating liquid nitrogen frozen after centrifuge washing, then low temperature drying 24 hours under low-temperature freeze-drying machine.
The calcining can be warming up to 300~600 DEG C under the heating rate of 10 DEG C/min.
Beneficial effects of the present invention:
1, calcining has easy to operate, Portable safety, low-temperature energy-saving, reproducible in hydrothermal synthesis and air of the invention
The advantages of.
2, product of the invention is the spherical porous V of the different-diameter size of high-purity2O5New pattern is lithium ion battery
In good anode material.
3, the present invention only can be obtained by different-diameter size precursor vanadic acid second two by controlling mixed solution mixing time
Alcohol ester (VEG) obtains spherical, porous V through calcining2O5New pattern, obtained spherical, porous V2O5New pattern is protected well
The sphere sizes of precursor vanadic acid ethylene glycol rouge have been stayed, therefore have had the characteristics that spherical diameter size is easily-controllable.
Detailed description of the invention
Fig. 1 is the XRD spectrum of the obtained spherical shape precursor VEG (vanadic acid ethylene glycol rouge) of embodiment 1.
Fig. 2 is that the SEM of the obtained spherical shape precursor VEG (vanadic acid ethylene glycol rouge) of embodiment 1 schemes.
Fig. 3 is the XRD spectrum of the obtained spherical shape precursor VEG (vanadic acid ethylene glycol rouge) of embodiment 2.
Fig. 4 is that the SEM of the obtained spherical shape precursor VEG (vanadic acid ethylene glycol rouge) of embodiment 2 schemes.
Fig. 5 is the XRD spectrum of the obtained spherical shape precursor VEG (vanadic acid ethylene glycol rouge) of embodiment 3.
Fig. 6 is that the SEM of the obtained spherical shape precursor VEG (vanadic acid ethylene glycol rouge) of embodiment 3 schemes.
Fig. 7 is the XRD spectrum of the obtained spherical shape precursor VEG (vanadic acid ethylene glycol rouge) of embodiment 4.
Fig. 8 is that the SEM of the obtained spherical shape precursor VEG (vanadic acid ethylene glycol rouge) of embodiment 4 schemes.
Fig. 9 is the XRD spectrum of the obtained spherical shape precursor VEG (vanadic acid ethylene glycol rouge) of embodiment 5.
Figure 10 is that the SEM of the obtained spherical shape precursor VEG (vanadic acid ethylene glycol rouge) of embodiment 5 schemes.
Figure 11 is the XRD spectrum of the obtained spherical shape precursor VEG (vanadic acid ethylene glycol rouge) of embodiment 6.
Figure 12 is that the SEM of the obtained spherical shape precursor VEG (vanadic acid ethylene glycol rouge) of embodiment 6 schemes.
Figure 13 is 7 products therefrom V of embodiment2O5XRD spectrum.
Figure 14 is 7 products therefrom V of embodiment2O5SEM figure.
Figure 15 is 8 products therefrom V of embodiment2O5SEM figure.
Specific embodiment
It is next combined with specific embodiments below that the present invention is further explained.Mainly illustrate the mixing time of mixed solution to precursor
(VEG) influence of spherical diameter size.
Examples 1 to 6 has specifically probed into influence of the mixing time of mixed solution to precursor VEG diameter dimension.Embodiment 7
~8 have probed into calcine spherical precursor in air and prepare spherical, porous V2O5Pattern, V2O5Spherical diameter size
It is identical as the spherical diameter size of precursor.
Embodiment 1
0.5849g ammonium metavanadate is taken to be dissolved in 200ml ethylene glycol beaker, it can after ammonium metavanadate and ethylene glycol are sufficiently mixed
Yellow floccule is obtained, 0.5212g hydroxylammonium chloride is then added in beaker and is placed on magnetic stirring apparatus and stirs, revolving speed setting
1000 revs/min, 30min is stirred at normal temperatures and pressures, and yellow floccule gradually becomes white, obtains the precursor of white flock.
Solution after mixing is transferred in the stainless steel hydrothermal reaction kettle of polytetrafluoroethyllining lining (packing ratio 80%), is placed in temperature
It is heated in the controllable heating furnace of degree intelligence, reaction condition are as follows: 160 DEG C of reaction temperature, after 15 hours reaction time natural cooling
To hydro-thermal product.Hydro-thermal product is centrifugally separating to obtain purple red precipitate, with deionized water and dehydrated alcohol centrifuge washing 5 times,
Precipitating liquid nitrogen frozen after centrifuge washing, then low temperature drying 24 hours under low-temperature freeze-drying machine again, obtain grey black
Powder.
The XRD spectra of the powder of grey black is as shown in Figure 1, parsing XRD spectra shows that the powder of prepared grey black produces
Object is precursor VEG (vanadic acid ethylene glycol rouge), and has good crystal structure.Prepared precursor VEG uses Magellan
400 type field emission scanning electron microscopes observe pattern, as shown in Fig. 2.Figure it is seen that prepared precursor VEG
Diameter size distribution at 1~3 μm.
Embodiment 2
Identical as the process of embodiment 1, only the hydro-thermal reaction time is 25 small to solution after mixing in a kettle
When, other conditions are constant.
The XRD spectra of the powder of obtained grey black is as shown in figure 3, parsing XRD spectra shows prepared grey black
Powdered product is precursor VEG (vanadic acid ethylene glycol rouge), and has good crystal structure.Prepared precursor VEG is used
Magellan 400 type field emission scanning electron microscope observes pattern, as shown in Figure 4.From fig. 4, it can be seen that prepared
The diameter size distribution of precursor VEG is at 1~3 μm.
Embodiment 3
Identical as the process of embodiment 1, only the hydro-thermal reaction time is 35 small to solution after mixing in a kettle
When, other conditions are constant.
The XRD spectra of the powder of obtained grey black is as shown in figure 5, parsing XRD spectra shows prepared grey black
Powdered product is precursor VEG (vanadic acid ethylene glycol rouge), and has good crystal structure.Prepared precursor VEG is used
Magellan 400 type field emission scanning electron microscope observes pattern, as shown in Figure 6.From fig. 6, it can be seen that prepared
The diameter dimension of precursor VEG is also distributed about 1~3 μm.
By Examples 1 to 3 it is found that in the case where the other variables of control are constant, when only changing the hydro-thermal reaction time, hydro-thermal
Reaction time does not influence substantially in 10~35 hours ranges, on the diameter dimension of precursor VEG.
Embodiment 4
The mixing time of embodiment 1 is revised as 2h, other conditions are constant.
The XRD spectra of the powder of grey black obtained is as shown in fig. 7, parsing XRD spectra shows prepared grey black
Powdered product is precursor VEG (vanadic acid ethylene glycol rouge), and has good crystal structure.Prepared precursor VEG is used
Magellan 400 type field emission scanning electron microscope observes pattern, as shown in Figure 8.As can be seen from Figure 8, prepared
Precursor VEG diameter size distribution at 3~5 μm.
Embodiment 5
The mixing time of embodiment 1 is revised as 4h, other conditions are constant.
The XRD spectra of the powder of grey black obtained is as shown in figure 9, parsing XRD spectra shows prepared grey black
Powdered product is precursor VEG (vanadic acid ethylene glycol rouge), and has good crystal structure.Prepared precursor VEG is used
Magellan 400 type field emission scanning electron microscope observes pattern, as shown in Figure 10.It can be seen from fig. 10 that made
The diameter size distribution of standby precursor VEG is at 6~10 μm.
Embodiment 6
The mixing time of embodiment 1 is revised as 8h, other conditions are constant.
The XRD spectra of the powder of grey black obtained is as shown in figure 11, and parsing XRD spectra shows prepared grey black
Powdered product be precursor VEG (vanadic acid ethylene glycol rouge), and have good crystal structure.Prepared precursor VEG is used
Magellan 400 type field emission scanning electron microscope observes pattern, as shown in figure 12.In figure 12 it can be seen that made
The diameter size distribution of standby precursor VEG is at 7~11 μm.
Experiment shows that the mixing time for changing mixed solution influences whether precursor in the case where controlling other variables
Diameter dimension, specifically: the diameter dimension of precursor VEG can increase with the increase of mixing time.
Embodiment 7
By such as precursor VEG (the vanadic acid ethylene glycol rouge) sample of preparation of embodiment 1, calcined in tube furnace.Calcination condition:
It is calcined under air, calcination temperature is 300 DEG C, and heating rate is 10 DEG C/min, and heating time is 4 hours, be can be obtained spherical, porous
V2O5New pattern.
The XRD spectra of product is as shown in figure 13, and parsing XRD spectra shows that prepared sample has good crystal knot
Structure, product are vanadic anhydride.Prepared sample is observed using 400 type field emission scanning electron microscope of Magellan
Pattern, as shown in figure 14.As can be seen from Figure 14, prepared V2O5For spherical porous pattern, and five oxidations two prepared
Vanadium remains the sphere sizes of precursor VEG.
Embodiment 8
By such as precursor VEG (the vanadic acid ethylene glycol rouge) sample of preparation of embodiment 1, calcined in tube furnace.Calcination condition:
It is calcined under air, calcination temperature is 600 DEG C, and heating rate is 10 DEG C/min, and heating time is 3 hours, be can be obtained spherical, porous
V2O5New pattern.
The XRD spectra of product is identical as Figure 13 of embodiment 7, illustrates that prepared sample is that have good crystal structure
Vanadic anhydride.Prepared sample observes pattern using 400 type field emission scanning electron microscope of Magellan, such as
Shown in Figure 15.As can be seen from Figure 15, prepared V2O5For spherical porous pattern, and the vanadic anhydride prepared retains
The sphere sizes of precursor VEG.
Experiment shows the spherical porous V prepared after calcining2O5Substantially the original pattern of precursor VEG is maintained, and is led to
It crosses to probe into and has found that the spherical diameter size of precursor VEG is under certain mixing time in the case where the other variables of control are constant
It can increase with the increase of mixing time.Therefore, available not by calcining the precursor VEG of different-diameter size in air
With the spherical porous V of diameter dimension2O5New pattern.
Claims (5)
1. a kind of prepare the spherical porous pattern V of different-diameter size2O5Method, prepare precursor vanadic acid ethylene glycol rouge, prepare ball
The porous pattern V of shape2O5Process；It is characterized in that,
The process for preparing precursor vanadic acid ethylene glycol rouge is that hydroxylamine hydrochloride is added after mixing ammonium metavanadate and ethylene glycol,
Obtain mixed solution, wherein the molar ratio of ammonium metavanadate and hydroxylamine hydrochloride is 2:3~3.1, mole of ammonium metavanadate and ethylene glycol
Than for 1:715~718；Mixed solution is transferred to reaction kettle polytetrafluoro after 1000~1500 revs/min are stirred 0.5~8 hour
In ethylene liner, reacted 10~35 hours under the conditions of 160~170 DEG C；Separation of solid and liquid obtains purple red precipitate, centrifuge washing,
Frozen drying obtains precursor vanadic acid ethylene glycol rouge；
The V for preparing spherical porous pattern2O5Process, be by 300~600 DEG C in air of precursor vanadic acid ethylene glycol rouge
Spherical, porous V is prepared in lower calcining 3~4 hours2O5Pattern.
2. the spherical porous pattern V of preparation different-diameter size according to claim 12O5Method, which is characterized in that institute
The ethylene glycol stated, density are 1.111~1.115g/ml.
3. the spherical porous pattern V of preparation different-diameter size according to claim 12O5Method, which is characterized in that institute
That states is transferred in reaction kettle polytetrafluoroethyllining lining, and packing ratio is 80% by volume.
4. the spherical porous pattern V of preparation different-diameter size according to claim 12O5Method, which is characterized in that institute
The centrifuge washing stated is to purple red precipitate deionized water and dehydrated alcohol centrifuge washing 5 times；The low temperature cold freeze-drying
It is dry, it is by the precipitating liquid nitrogen frozen after centrifuge washing, then low temperature drying 24 hours under low-temperature freeze-drying machine.
5. the spherical porous pattern V of preparation different-diameter size according to claim 1,2,3 or 42O5Method, feature
It is, the calcining, is to be warming up to 300~600 DEG C under the heating rate of 10 DEG C/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110205803A (en) * | 2019-05-30 | 2019-09-06 | 四川大学 | A kind of multivalent state barium oxide flexible electrode preparation method |
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| CN110205803A (en) * | 2019-05-30 | 2019-09-06 | 四川大学 | A kind of multivalent state barium oxide flexible electrode preparation method |
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Application publication date: 20190308 |