CN108117099A - A kind of spherical VOOH powders of stub self assembly and preparation method and application - Google Patents
A kind of spherical VOOH powders of stub self assembly and preparation method and application Download PDFInfo
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Abstract
A kind of spherical VOOH powders of stub self assembly and preparation method and application, solution A is obtained by being dissolved under sodium metavanadate and thioacetamide magnetic agitation in deionized water；The pH value of solution A is adjusted to 12.8~13.2, obtains solution B；Solution B is transferred to hydro-thermal reaction in hydro-thermal reaction liner；Drying obtains the spherical VOOH powders of stub self assembly after hydro-thermal reaction.The spherical VOOH powders of stub self assembly have uniform three-level self-assembled structures, by extra small nano-particles self assemble into sub-micron stub, sub-micron stub is self-assembled into micron ball, a diameter of 100~500nm of VOOH stubs, length is 200~1000nm, assembled by nanometer little particle, intersected in six side's shapes, part stub, part stub ruptures, the ball of a diameter of 2~5 μm of the spherical VOOH of stub self assembly.The spherical VOOH powders of stub self assembly are in the application of sodium/lithium/Magnesium ion battery, ultracapacitor and optical electrical catalytic field.VOOH can be made to show higher capacity, faster electrochemical reaction power and superior high rate performance.
Description
Technical field
The present invention relates to a kind of preparation methods of barium oxide, and in particular to a kind of spherical VOOH powders of stub self assembly and
Preparation method and use.
Background technology
Due to its unique electronics and optical characteristics, the barium oxide with changeable valency has been widely regarded as a kind of non-
Normal promising transition metal oxide.At present, substantial amounts of scholar's system research V2O5And VO2, include their synthesis side
Method, such as reverse micelle transformation approach, sol-gel method, hydro-thermal method, electrodeposition process, nanostructured, such as nanotube, nano wire, Nanowire
Dimension, nanobelt, nanometer rods and meso-hole structure, these make V2O5And VO2In sensor, transfer optics, optical storage of data matchmaker
Be situated between and the fields such as electrode material in be widely applied that [Wu C.Z, Xie Y, Lei L.Y, wait .Synthesis of New-
Phased VOOH Hollow“Dandelions”and Their Application in Lithium‐Ion Batteries
[J].Advanced Materials,2006,18(13):1727-1732.]。
The characteristics of transition metal barium oxide, causes the extensive concern of people, these compounds have open stratiform knot
Structure, generally strong covalent bond in layer, interlayer is weak Van der Waals force or hydrogen bond, can be embedded in atom or molecule, and V
Oxidation state is various (mainly in V5+~V2+Between), there is good reactivity, the capacity volume variance between them is little, has
The metallic compounds of a variety of mixed valences exist.Compared with other positive electrodes, the great advantage of barium oxide be have compared with
High specific capacity shows very strong attraction, and people are to oxyvanadium compound V2O5、V6O13、VO2、V3O7、V6O14、V4O9、
V2O3Cathode material as lithium ion battery has carried out some research [vanadium oxygen in Chen Changguo, Liu Yuping, Li Lan lithium ion batteries
Present Research [J] Journal of Inorganic Materials of compound electrode material, 2004,19 (6):1225-1230.].In addition, barium oxide is
A kind of typical layer structure material, ion deinsertion space is big, theoretical capacity is high, cheap, rich reserves, is to have very much
The cell positive material of prospect, has been widely studied.Barium oxide has changeable valence state and compound, is reacted by polyelectron
High memory capacity can be obtained, abundant layer structure provides for the sodium ion storage of high power capacity may [Wei's pond dragon, Jiang's week
Sun, Tan Shuanshuan wait application [J] the silicate journals of barium oxide nano materials in sodium-ion battery, 2016,44 (5):
693-706.]。
However, the report at present on VOOH is seldom, the report having had is also that hollow microsphere is synthesized by two-step process,
Reaction process is complex.
The content of the invention
It is an object of the invention to provide spherical VOOH powders of a kind of stub self assembly and its preparation method and application, prepare
Method is easy to operate, and reaction temperature i.e. available by a traditional step hydro-thermal is low, reaction time is short, VOOH powders obtained
Chemical constituent is homogeneous, purity is high, pattern is uniform and has self-assembled structures.
In order to achieve the above objectives, the preparation method that the present invention uses includes：
Step 1：Take and be dissolved in 55 under 0.8~1.2g sodium metavanadates and 2.8~3.2g thioacetamide magnetic agitations~
Solution A is obtained in 65ml deionized waters；
Step 2：The NaOH solution that 0.7~0.9mol/L is added dropwise dropwise into solution A under magnetic stirring adjusts solution A
PH value to 12.8~13.2, obtain solution B；
Step 3：Solution B is transferred in hydro-thermal reaction liner, outer kettle is installed additional and is placed in homogeneous reaction instrument contorted
Under state 175~185 DEG C of progress hydro-thermal reactions are heated to from room temperature；
Step 4：Terminate after hydro-thermal reaction and take out reaction product after natural cooling, collected after washing, alcohol are washed, and
Drying obtains the spherical VOOH powders of stub self assembly under conditions of 55~65 DEG C.
The magnetic agitation rotating speed of the step 1 is 400~600r/min, and mixing time is 55~65min.
The rate of addition of the step 2 NaOH solution is 0.08~0.12ml/min, drips previous drop NaOH solution,
Stirring is after solution ph is stablized, then instills next drop NaOH solution, until reacting liquid pH value is adjusted to 12.8~13.2.
The packing ratio that the step 3 solution B is transferred to hydro-thermal reaction liner is 55~65%.
The rotating speed of the step 3 hydro-thermal reaction is 5~8r/min
The step 3 the hydro-thermal reaction time is 23.5~24.5h.
The washing of the step 4, alcohol is washed to be washed 3-6 times respectively using filtering and washing or centrifuge washing, is collected using suction filtration
It collects or is collected by centrifugation.
The step 4 drying time is 11~13h.
The spherical VOOH powders of the stub self assembly as made of method made above have uniform three-level self-assembled structures, by
For extra small nano-particles self assemble into sub-micron stub, sub-micron stub is self-assembled into micron ball, VOOH stubs a diameter of 100~
500nm, length are 200~1000nm, are assembled by nanometer little particle, in six side's shapes, part stub intersect, part stub is broken
It splits, the ball of a diameter of 2~5 μm of the spherical VOOH of stub self assembly.
The spherical VOOH powders of stub self assembly are in sodium/lithium/Magnesium ion battery, ultracapacitor and optical electrical catalytic field
Using.VOOH powders have relatively low crystallinity, can be Mg2+/Na+/Li+Storage more active sites are provided, also may be used
More passages are provided to enter for these ions inside lattice entity, and then VOOH can be made to show higher capacity, more
Fast electrochemical reaction power and superior high rate performance.
Compared with the prior art, the present invention at least has the advantages that：
(1) present invention is prepared for VOOH powders using a step low-temperature hydrothermal synthetic method, the method overcome two-step method synthesis
The shortcomings that complicated, and large scale equipment and harsh reaction condition is not required, without pattern controlling agent, raw material is cheap and easy to get, cost
Low, yield is high, environmentally friendly without post-processing, can be suitble to mass produce.
(2) this method is simple for process easily-controllable, and the VOOH powders chemical composition and pattern of preparation are homogeneous, purity is higher and has
Excellent chemical property.
(3) sodium metavanadate and thioacetamide are mixed to solution after being dissolved in deionized water before the reaction and clarify shape in half
State, at this moment the vanadium source in solution and sulphur source be in specific state, this state is self-assembled into six sides Asia for nanometer little particle
Micron bar and then self assembly are in that the appearance structure of micron ball plays very crucial effect.This structure is in clear solution state
Under can not be formed.
(4) during entire pH is adjusted, the concentration of NaOH, rate of addition, dropwise addition process and the pH value that finally controls for
The synthesis of the spherical VOOH powders of pure phase stub self assembly has conclusive effect.First, excessively high NaOH concentration and too fast
Rate of addition, may cause the reaction of local reaction liquid, and then dephasign is introduced in final product, too low NaOH concentration and
It crosses slow rate of addition and is unfavorable for VO+Formation, and then the formation of VOOH can be influenced.Secondly, the excessively high pH value of end reaction liquid
The introducing of other oxide dephasigns is had, too low pH value is then unfavorable for providing more OH-, and then it is unfavorable for the shape of VOOH
Into.
(5) the packing ratio requirement of hydro-thermal reaction is strict controlled in 55~65% in this method, and excessively high packing ratio can make instead
It should be under higher pressure, so as to cause the appearance of vanadic sulfide, too low packing ratio can be such that reaction is under relatively low pressure,
So as to be unfavorable for the formation of VOOH.
(6) drying temperature of product and time will be strict controlled in 55~65 DEG C and 11~13h, excessively high temperature in this method
Degree and long time will make VOOH lose OH-, too low drying temperature and too short drying time are then unfavorable for moisture
Removal.
(7) VOOH powders prepared by this method have unique three-level self-assembled structures, i.e., by extra small nano particle from group
Sub-micron stub is dressed up, then sub-micron stub is self-assembled into micron ball again.A diameter of 100~500nm of VOOH stubs, length
For 200~1000nm, and assembled by nanometer little particle, intersected in six side's shapes, part stub, part stub ruptures.It is short
The spherical VOOH of stick self assembly is mostly 2~5 μm of ball for diameter.The structure of exactly this uniqueness is it in sodium/lithium/magnesium ion
The application of battery, ultracapacitor and optical electrical catalytic field provides guarantee.
(8) VOOH powders prepared by this method have relatively low crystallinity, can be Mg2+/Na+/Li+Storage provide
More active sites, or these ions, which enter, provides more passages inside lattice entity, and then can make VOOH
Show higher capacity, faster electrochemical reaction power and superior high rate performance.
Description of the drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of VOOH nano-powders prepared by the embodiment of the present invention 1.
(other conditions and 1 complete phase of embodiment when reaction-filling ratio in embodiment 1 is adjusted to 70% by Fig. 2 for the present invention
Together), the XRD spectrum of product is prepared.
(other conditions and 1 complete phase of embodiment when reaction-filling ratio in embodiment 1 is adjusted to 50% by Fig. 3 for the present invention
Together), the XRD spectrum of product is prepared.
Fig. 4 is low power scanning electron microscope (SEM) photo of VOOH nano-powders prepared by the embodiment of the present invention 1.
Fig. 5 is the high power SEM photograph of VOOH nano-powders prepared by the embodiment of the present invention 1.
Fig. 6 is the SEM photograph of VOOH nano-powders more high power prepared by the embodiment of the present invention 1.
Fig. 7 is low power transmission electron microscope (TEM) figure of VOOH sub-micron stubs prepared by the embodiment of the present invention 1.
Fig. 8 is the high power TEM figures of VOOH sub-micron stubs prepared by the embodiment of the present invention 1.
Fig. 9 is the high-resolution TEM figures of VOOH sub-micron stubs prepared by the embodiment of the present invention 1.
Figure 10 is that (other conditions are with implementing when the concentration of sodium hydroxide in the embodiment of the present invention 1 is adjusted to 1.2mol/L
Example 1 is identical), the SEM photograph of products therefrom.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Embodiment 1：
Step 1：1.0g sodium metavanadates and 3.0g thioacetamides is taken to be dissolved in 600r/min magnetic agitations 60min
Solution A is obtained in 60ml deionized waters；
Step 2：The NaOH of 0.8mol/L, the rate of addition of NaOH solution is added dropwise dropwise into solution A under magnetic stirring
For 0.08ml/min, previous drop NaOH solution is dripped, after stirring is until solution ph stablizes, then to instill next drop NaOH molten
Liquid until reacting liquid pH value is adjusted to 13, obtains solution B；
Step 3：Solution B is transferred in hydro-thermal reaction liner by 60% packing ratio, the outer kettle of installation, which is placed on, to be contrary
Ying Yizhong is heated to 180 DEG C from room temperature under 5r/min rotation status and carries out hydro-thermal reaction for 24 hours；
Step 4：Terminate after hydro-thermal reaction and take out reaction product after natural cooling, used by the way of filtering and washing
Collected by suction after washing, alcohol wash 3 times, and dry 12h under conditions of 60 DEG C and obtain the spherical VOOH powders of stub self assembly.
From figure 1 it appears that all diffraction maximums both point to VOOH powders, there is no the appearance of other miscellaneous peaks, because
This VOOH powder has higher object phase purity.Meanwhile crude back end illustrates that the VOOH powders have relatively low crystallinity.
From figure 2 it can be seen that when increasing reaction-filling ratio to 70%, the product of synthesis is mainly VS2, while also companion
With the generation of dephasign S simple substance.Therefore, excessively high packing ratio is unfavorable for the synthesis of VOOH.
From figure 3, it can be seen that when reducing reaction-filling ratio to 50%, the product of synthesis is mainly sulphur simple substance, not
There is the synthesis of VOOH.Therefore, synthesis of the too low reaction-filling than being also unfavorable for VOOH.
Figure 4, it is seen that the VOOH has uniform pattern, it is all spherical into micron, and the mutual heap of these micron balls
It stacks.
From figure 5 it can be seen that the scale of micron ball is 2~5 μm, and it is by a diameter of 100~500nm, and length is
The sub-micro stick self assembly of 200~1000nm forms.
As can be seen from Figure 6 sub-micrometer rod is assembled by nanometer little particle, and in six side's shapes, part stub intersects,
Part stub rupture.
It can be seen from figure 7 that the VOOH sub-micron stub is solid construction.
As can be seen from Figure 8, which formed by extra small nano-particles self assemble.
It can be seen in figure 9 that the diffraction fringe of VOOH has relatively low clarity, show that the VOOH has relatively low knot
Brilliant degree.
It can be seen from fig. 10 that products therefrom is by VOOH micron bars and VS2Nanometer sheet two parts form.Therefore, it is higher
NaOH concentration can make to generate substantial amounts of VS in synthetic product2Dephasign is unfavorable for the synthesis of pure phase VOOH.
Embodiment 2：
Step 1：0.8g sodium metavanadates and 2.9g thioacetamides is taken to be dissolved in 500r/min magnetic agitations 55min
Solution A is obtained in 55ml deionized waters；
Step 2：The NaOH of 0.7mol/L, the rate of addition of NaOH solution is added dropwise dropwise into solution A under magnetic stirring
For 0.09ml/min, previous drop NaOH solution is dripped, after stirring is until solution ph stablizes, then to instill next drop NaOH molten
Liquid until reacting liquid pH value is adjusted to 12.8, obtains solution B；
Step 3：Solution B is transferred in hydro-thermal reaction liner by 55% packing ratio, the outer kettle of installation, which is placed on, to be contrary
Ying Yizhong is heated to 183 DEG C from room temperature under 7r/min rotation status and carries out hydro-thermal reaction 23.5h；
Step 4：Terminate after hydro-thermal reaction and take out reaction product after natural cooling, be washed with water by the way of centrifugation,
Alcohol is collected by centrifugation after washing 5 times, and dries 13h under conditions of 55 DEG C and obtain the spherical VOOH powders of stub self assembly.
Embodiment 3：
Step 1：1.1g sodium metavanadates and 2.8g thioacetamides is taken to be dissolved in 400r/min magnetic agitations 58min
Solution A is obtained in 58ml deionized waters；
Step 2：The NaOH of 0.9mol/L, the rate of addition of NaOH solution is added dropwise dropwise into solution A under magnetic stirring
For 0.10ml/min, previous drop NaOH solution is dripped, after stirring is until solution ph stablizes, then to instill next drop NaOH molten
Liquid until reacting liquid pH value is adjusted to 13.1, obtains solution B；
Step 3：Solution B is transferred in hydro-thermal reaction liner by 63% packing ratio, the outer kettle of installation, which is placed on, to be contrary
Ying Yizhong is heated to 185 DEG C from room temperature under 6r/min rotation status and carries out hydro-thermal reaction 23.5h；
Step 4：Terminate after hydro-thermal reaction and take out reaction product after natural cooling, used by the way of filtering and washing
Collected by suction after washing, alcohol wash 6 times, and dry 11h under conditions of 63 DEG C and obtain the spherical VOOH powders of stub self assembly.
Embodiment 4：
Step 1：0.9g sodium metavanadates and 3.2g thioacetamides is taken to be dissolved in 450r/min magnetic agitations 65min
Solution A is obtained in 65ml deionized waters；
Step 2：The NaOH of 0.9mol/L, the rate of addition of NaOH solution is added dropwise dropwise into solution A under magnetic stirring
For 0.12ml/min, previous drop NaOH solution is dripped, after stirring is until solution ph stablizes, then to instill next drop NaOH molten
Liquid until reacting liquid pH value is adjusted to 12.9, obtains solution B；
Step 3：Solution B is transferred in hydro-thermal reaction liner by 58% packing ratio, the outer kettle of installation, which is placed on, to be contrary
Ying Yizhong is heated to 175 DEG C from room temperature under 8r/min rotation status and carries out hydro-thermal reaction 24.5h；
Step 4：Terminate after hydro-thermal reaction and take out reaction product after natural cooling, be washed with water by the way of centrifugation,
Collected by suction after alcohol washes 4 times, and dry 13h under conditions of 58 DEG C and obtain the spherical VOOH powders of stub self assembly.
Embodiment 5：
Step 1：1.2g sodium metavanadates and 3.1g thioacetamides is taken to be dissolved in 550r/min magnetic agitations 63min
Solution A is obtained in 63ml deionized waters；
Step 2：The NaOH of 0.7mol/L, the rate of addition of NaOH solution is added dropwise dropwise into solution A under magnetic stirring
For 0.11ml/min, previous drop NaOH solution is dripped, after stirring is until solution ph stablizes, then to instill next drop NaOH molten
Liquid until reacting liquid pH value is adjusted to 13.2, obtains solution B；
Step 3：Solution B is transferred in hydro-thermal reaction liner by 65% packing ratio, the outer kettle of installation, which is placed on, to be contrary
Ying Yizhong is heated to 178 DEG C from room temperature under 6r/min rotation status and carries out hydro-thermal reaction for 24 hours；
Step 4：Terminate after hydro-thermal reaction and take out reaction product after natural cooling, used by the way of filtering and washing
Washing, alcohol are collected by centrifugation after washing 5 times, and dry 11h under conditions of 65 DEG C and obtain the spherical VOOH powders of stub self assembly.
Claims (10)
1. a kind of spherical VOOH raw powder's production technologies of stub self assembly, it is characterised in that comprise the following steps：
Step 1：It takes and is dissolved in 55~65ml under 0.8~1.2g sodium metavanadates and 2.8~3.2g thioacetamide magnetic agitations
Solution A is obtained in ionized water；
Step 2：The NaOH solution that 0.7~0.9mol/L is added dropwise dropwise into solution A under magnetic stirring adjusts the pH of solution A
Value obtains solution B to 12.8~13.2；
Step 3：Solution B is transferred in hydro-thermal reaction liner, outer kettle is installed additional and is placed in homogeneous reaction instrument under rotation status
175~185 DEG C of progress hydro-thermal reactions are heated to from room temperature；
Step 4：Terminate after hydro-thermal reaction and take out reaction product after natural cooling, collected after washing, alcohol are washed, and 55
Drying obtains the spherical VOOH powders of stub self assembly under conditions of~65 DEG C.
2. the spherical VOOH raw powder's production technologies of stub self assembly according to claim 1, it is characterised in that：The step
One magnetic agitation rotating speed is 400~600r/min, and mixing time is 55~65min.
3. the spherical VOOH raw powder's production technologies of stub self assembly according to claim 1, it is characterised in that：The step
The rate of addition of two NaOH solutions is 0.08~0.12ml/min, drips previous drop NaOH solution, stirring is until solution ph
After stabilization, then next drop NaOH solution is instilled, until reacting liquid pH value is adjusted to 12.8~13.2.
4. the spherical VOOH raw powder's production technologies of stub self assembly according to claim 1, it is characterised in that：The step
The packing ratio that three solution Bs are transferred to hydro-thermal reaction liner is 55~65%.
5. the spherical VOOH raw powder's production technologies of stub self assembly according to claim 1, it is characterised in that：The step
The rotating speed of three hydro-thermal reactions is 5~8r/min.
6. the spherical VOOH raw powder's production technologies of stub self assembly according to claim 1, it is characterised in that：The step
Three the hydro-thermal reaction times are 23.5~24.5h.
7. the spherical VOOH raw powder's production technologies of stub self assembly according to claim 1, it is characterised in that：The step
Four washing, alcohol is washed to be washed 3-6 times respectively using filtering and washing or centrifuge washing, is collected using collected by suction or is collected by centrifugation.
8. the spherical VOOH raw powder's production technologies of stub self assembly according to claim 1, it is characterised in that：The step
Four drying times are 11~13h.
9. a kind of spherical VOOH powders of stub self assembly made of preparation method as described in claim 1, it is characterised in that：
VOOH powders have uniform three-level self-assembled structures, by extra small nano-particles self assemble into sub-micron stub, sub-micron stub
Micron ball, a diameter of 100~500nm of VOOH stubs are self-assembled into, length is 200~1000nm, is assembled by nanometer little particle
It forms, intersect in six side's shapes, part stub, part stub ruptures, the ball of a diameter of 2~5 μm of the spherical VOOH of stub self assembly.
10. a kind of spherical VOOH powders of stub self assembly as claimed in claim 9 are in sodium/lithium/Magnesium ion battery, super capacitor
The application of device and optical electrical catalytic field.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113184906A (en) * | 2021-05-13 | 2021-07-30 | 陕西科技大学 | One-step hydrothermal method for preparing V2O3Method of nanosphere |
| CN115092961A (en) * | 2022-07-14 | 2022-09-23 | 贵州大学 | Preparation method and application of hydroxyl vanadium oxide with hollow spherical shell structure |
| CN115611310A (en) * | 2022-10-08 | 2023-01-17 | 武汉科技大学 | Method for preparing high-purity vanadium pentoxide by using vanadium-containing solution |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107381636A (en) * | 2017-07-11 | 2017-11-24 | 陕西科技大学 | A kind of vanadic sulfide powder of nano-particles self assemble three dimensional micron cauliflower-shaped four and its preparation method and application |
-
2017
- 2017-12-22 CN CN201711403791.2A patent/CN108117099B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107381636A (en) * | 2017-07-11 | 2017-11-24 | 陕西科技大学 | A kind of vanadic sulfide powder of nano-particles self assemble three dimensional micron cauliflower-shaped four and its preparation method and application |
Non-Patent Citations (4)
| Title |
|---|
| CHANGZHENG WU ET AL.: "New phase hollandite-type VOOH quadrangular nanorods: a new smart electrical switch material", 《CHEM. COMMUN》 * |
| CHANGZHENG WU ET AL.: "Synthesis of New-Phased VOOH Hollow "Dandelions" and Their Application in Lithium-Ion Batteries", 《ADV. MATER》 * |
| JIE SHAO ET AL.: "Low crystallinity VOOH hollow microspheres as an outstanding high-rate and long-life cathode for sodium ion batteries", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| WENBIN LI ET AL.: "Facile in situ synthesis of crystalline VOOH-coated VS2 microflowers with superior sodium storage performance", 《J. MATER. CHEM. A》 * |
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| CN115092961A (en) * | 2022-07-14 | 2022-09-23 | 贵州大学 | Preparation method and application of hydroxyl vanadium oxide with hollow spherical shell structure |
| CN115092961B (en) * | 2022-07-14 | 2023-12-22 | 贵州大学 | Preparation method and application of hollow spherical shell structured vanadium oxyhydroxide |
| CN115611310A (en) * | 2022-10-08 | 2023-01-17 | 武汉科技大学 | Method for preparing high-purity vanadium pentoxide by using vanadium-containing solution |
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