CN108117099B - Short-rod self-assembled spherical VOOH powder and preparation method and application thereof - Google Patents

Short-rod self-assembled spherical VOOH powder and preparation method and application thereof Download PDF

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CN108117099B
CN108117099B CN201711403791.2A CN201711403791A CN108117099B CN 108117099 B CN108117099 B CN 108117099B CN 201711403791 A CN201711403791 A CN 201711403791A CN 108117099 B CN108117099 B CN 108117099B
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黄剑锋
***
曹丽云
冯亮亮
闻稼宝
任一杰
刘倩倩
张芝
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Shaanxi University of Science and Technology
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    • C01G31/00—Compounds of vanadium
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    • C01—INORGANIC CHEMISTRY
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    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
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    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
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    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer

Abstract

A short-rod self-assembly spherical VOOH powder and a preparation method and application thereof are disclosed, sodium metavanadate and thioacetamide are dissolved in deionized water under magnetic stirring to obtain a solution A; adjusting the pH value of the solution A to obtain a solution B; transferring the solution B to a hydrothermal reaction lining for hydrothermal reaction; and drying after the hydrothermal reaction is finished to obtain short-rod self-assembled spherical VOOH powder. The short rod self-assembly spherical VOOH powder has an even three-stage self-assembly structure, the submicron short rods are self-assembled by ultra-small nano particles and self-assembled into the micron balls, the diameter of each VOOH short rod is 100-500 nm, the length of each VOOH short rod is 200-1000 nm, each VOOH short rod is assembled by nano particles and is hexagonal, part of the VOOH short rods are crossed, part of the VOOH short rods are broken, and the diameter of the short rod self-assembly spherical VOOH is 2-5 mu m. The short-rod self-assembled spherical VOOH powder is applied to the fields of sodium/lithium/magnesium ion batteries, super capacitors and photo/electro-catalysis.

Description

Short-rod self-assembled spherical VOOH powder and preparation method and application thereof
Technical Field
The invention relates to a preparation method of vanadium oxide, in particular to short-rod self-assembled spherical VOOH powder and a preparation method and application thereof.
Background
Vanadium oxide having multiple valence changes has been widely recognized as a very promising transition metal oxide due to its unique electronic and optical properties. At present, a large number of student systems have studied V2O5And VO2Including their synthesis methods such as reverse micelle transfer, sol-gel, hydrothermal, electrodeposition, nanostructures such as nanotubes, nanowires, nanofibers, nanoribbons, nanorods and mesoporous structures, which make V2O5And VO2Has been widely used in the fields of sensors, optical conversion devices, optical data storage media, electrode materials, and the like [ Wu C.Z, Xie Y, Lei L.Y, et al Synthesis of New-Phased VOOH Hollow "Dandelions" and the same Application in Lithium-Ion Batteries [ J].Advanced Materials,2006,18(13):1727-1732.]。
The characteristics of transition metal vanadium oxides have attracted much attention, these compounds have an open layered structure, generally strong covalent bonds in the layers, weak van der waals forces or hydrogen bonds between the layers, and can be inserted into atoms or molecules, and the oxidation state of V is diverse (mainly in V)5+～V2+In between) has good reactivity, the energy difference between them is not large, and metallic compounds with various mixed valence states exist. The most important advantages of vanadium oxide compared with other anode materials are that the vanadium oxide has higher specific capacity and shows strong attraction, and people already aim at vanadium oxide compound V2O5、V6O13、VO2、V3O7、V6O14、V4O9、V2O3Some studies have been conducted as cathode materials for lithium ion batteries [ Chengchang, Liuyumna, Lilan ] current research situation of vanadium oxide electrode materials in lithium ion batteries [ J]Journal of inorganic materials 2004,19(6): 1225-.]. In addition, vanadium oxide is a typical layered structure material, has a large ion-deintercalation space, a high theoretical capacity, a low price and a rich reserve, is a battery cathode material with great prospect, and has been widely researched. Vanadium oxide has changeable valence and compound, high storage capacity can be obtained through multi-electron reaction, rich layered structure provides possibility for high-capacity sodium ion storage [ Weiqilong, Jiang Zhou Yang, Tan Shuangshuang, etc.. application of vanadium oxide nano material in sodium ion battery [ J]The silicate bulletin, 2016,44(5): 693-.]。
However, few reports on VOOH exist, and the synthesis of hollow microspheres by a two-step method is also reported, and the reaction process is complicated.
Disclosure of Invention
The invention aims to provide short-rod self-assembled spherical VOOH powder and a preparation method and application thereof, wherein the preparation method is simple to operate, can be obtained by traditional one-step hydrothermal method, and has the advantages of low reaction temperature, short reaction period, uniform chemical components, high purity, uniform appearance and self-assembled structure.
In order to achieve the above purpose, the preparation method adopted by the invention comprises the following steps:
the method comprises the following steps: dissolving 0.8-1.2 g of sodium metavanadate and 2.8-3.2 g of thioacetamide in 55-65 ml of deionized water under magnetic stirring to obtain a solution A;
step two: dropwise adding 0.7-0.9 mol/L NaOH solution into the solution A under magnetic stirring to adjust the pH value of the solution A to 12.8-13.2, and obtaining solution B;
step three: transferring the solution B into a hydrothermal reaction lining, adding an outer kettle, placing the outer kettle into a homogeneous phase reactor, and heating the solution B to 175-185 ℃ from room temperature under a rotating state to perform hydrothermal reaction;
step four: and after the hydrothermal reaction is finished and the reaction product is naturally cooled, taking out the reaction product, washing with water and alcohol, collecting the reaction product, and drying the reaction product at the temperature of 55-65 ℃ to obtain the short-rod self-assembled spherical VOOH powder.
The rotating speed of the magnetic stirring in the first step is 400-600 r/min, and the stirring time is 55-65 min.
And secondly, dropwise adding the NaOH solution at the speed of 0.08-0.12 ml/min, stirring until the pH value of the solution is stable, and then dropwise adding the next NaOH solution until the pH value of the reaction solution is adjusted to 12.8-13.2.
And the filling ratio of the solution B transferred to the hydrothermal reaction lining in the third step is 55-65%.
The rotating speed of the hydrothermal reaction in the third step is 5-8 r/min
The hydrothermal reaction time of the third step is 23.5-24.5 h.
And step four, washing with water, washing with alcohol by adopting suction filtration washing or centrifugal washing for 3-6 times respectively, and collecting by adopting suction filtration collection or centrifugal collection.
And the drying time of the fourth step is 11-13 h.
The short rod self-assembly spherical VOOH powder prepared by the preparation method has a uniform three-stage self-assembly structure, the submicron short rods are self-assembled by ultra-small nano particles and are self-assembled into micron balls, the diameter of each VOOH short rod is 100-500 nm, the length of each VOOH short rod is 200-1000 nm, each VOOH short rod is assembled by small nano particles and is hexagonal, part of short rods are crossed, part of short rods are broken, and the diameter of each short rod self-assembly spherical VOOH is 2-5 mu m.
The short-rod self-assembled spherical VOOH powder is applied to the fields of sodium/lithium/magnesium ion batteries, super capacitors and photo/electro-catalysis. The VOOH powder has low crystallinity, and can be Mg2+/Na+/Li+The storage of the organic silicon compound provides more active sites, and also provides more channels for the ions to enter the interior of the crystal lattice entity, so that VOOH can show higher capacity, faster electrochemical reaction power and more excellent rate performance.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) the VOOH powder is prepared by adopting a one-step low-temperature hydrothermal synthesis method, the method overcomes the defect of complex two-step synthesis, does not need large-scale equipment and harsh reaction conditions, does not need a morphology control agent, has cheap and easily obtained raw materials, low cost and high yield, does not need post-treatment, is environment-friendly, and can be suitable for large-scale production.
(2) The method has simple and easily-controlled process, and the prepared VOOH powder has uniform chemical composition and appearance, higher purity and excellent electrochemical performance.
(3) Before the reaction, sodium metavanadate and thioacetamide are mixed and dissolved in deionized water, then the solution is in a semi-clear state, and a vanadium source and a sulfur source in the solution are in a specific state, and the state plays a very key role in the self-assembly of nano-particles into a hexagonal submicron rod and then a morphology structure of a microsphere. This structure is not formed in a clear solution state.
(4) In the whole pH adjusting process, the concentration, the dripping speed, the dripping process and the finally controlled pH value of NaOH have a decisive effect on the synthesis of the pure-phase short-rod self-assembled spherical VOOH powder. Firstly, too high NaOH concentration and too fast drop acceleration may cause local reaction of the reaction solution, which in turn may be introduced into the final productImpure phase, too low NaOH concentration and too slow dripping acceleration are not beneficial to VO+Which in turn affects the formation of VOOH. Secondly, the final reaction solution with too high pH value can introduce other oxide impurity phase, while the too low pH value is not favorable for providing more OH-And thus adversely affect the formation of VOOH.
(5) In the method, the filling ratio of the hydrothermal reaction is strictly controlled to be 55-65%, too high filling ratio can enable the reaction to be under higher pressure, so that vanadium sulfide is generated, and too low filling ratio can enable the reaction to be under lower pressure, so that VOOH is not favorably formed.
(6) In the method, the drying temperature and time of the product are strictly controlled to be 55-65 ℃ and 11-13 h, and the excessive temperature and the excessive time can cause VOOH to lose OH-Too low a drying temperature and too short a drying time are disadvantageous for the removal of moisture.
(7) The VOOH powder prepared by the method has a unique three-stage self-assembly structure, namely, the submicron short rods are self-assembled by the ultra-small nano particles and then self-assembled into the micron balls. The VOOH short rods have the diameter of 100-500 nm and the length of 200-1000 nm, are assembled by nano small particles, and are hexagonal, part of the short rods are crossed, and part of the short rods are broken. The short-rod self-assembled spherical VOOH is mostly a sphere with the diameter of 2-5 μm. It is this unique structure that provides guarantee for its application in sodium/lithium/magnesium ion battery, ultracapacitor and light/electro-catalysis field.
(8) The VOOH powder prepared by the method has low crystallinity, and can be Mg2+/Na+/Li+The storage of the organic silicon compound provides more active sites, and also provides more channels for the ions to enter the interior of the crystal lattice entity, so that VOOH can show higher capacity, faster electrochemical reaction power and more excellent rate performance.
Drawings
Fig. 1 is an X-ray diffraction (XRD) pattern of VOOH nano powder prepared in example 1 of the present invention.
FIG. 2 is an XRD pattern of a product prepared by adjusting the reaction packing ratio of example 1 to 70% in the present invention (otherwise, exactly the same conditions as example 1).
FIG. 3 is an XRD pattern of a product prepared by adjusting the reaction packing ratio of example 1 to 50% in the present invention (otherwise, exactly the same conditions as example 1).
FIG. 4 is a Scanning Electron Microscope (SEM) image of VOOH nanopowder prepared in example 1 of the present invention.
Fig. 5 is a high-magnification SEM photograph of VOOH nanopowder prepared in example 1 of the present invention.
Fig. 6 is a SEM photograph of VOOH nano powder prepared in example 1 of the present invention at a higher magnification.
FIG. 7 is a low power Transmission Electron Microscope (TEM) image of VOOH submicron rods prepared in example 1 of the present invention.
FIG. 8 is a high power TEM image of VOOH submicron rods prepared in example 1 of the present invention.
FIG. 9 is a high resolution TEM image of VOOH submicron rods prepared in example 1 of the present invention.
FIG. 10 is an SEM photograph of a product obtained when the concentration of sodium hydroxide in example 1 of the present invention was adjusted to 1.2mol/L (otherwise, exactly the same conditions as in example 1).
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1:
the method comprises the following steps: dissolving 1.0g of sodium metavanadate and 3.0g of thioacetamide in 60ml of deionized water by magnetic stirring at the speed of 600r/min for 60min to obtain a solution A;
step two: dropwise adding 0.8mol/L NaOH into the solution A under magnetic stirring, wherein the dropping speed of the NaOH solution is 0.08ml/min, after the previous drop of the NaOH solution is added, stirring until the pH value of the solution is stable, and then adding the next drop of the NaOH solution until the pH value of the reaction solution is adjusted to 13 to obtain a solution B;
step three: transferring the solution B into a hydrothermal reaction lining according to the filling ratio of 60%, adding an outer kettle, placing the outer kettle in a homogeneous reactor, and heating the mixture from room temperature to 180 ℃ in a rotating state of 5r/min to perform hydrothermal reaction for 24 hours;
step four: and after the hydrothermal reaction is finished and the reaction product is naturally cooled, taking out the reaction product, washing the reaction product by water and alcohol for 3 times in a suction filtration washing mode, then carrying out suction filtration and collection, and drying the reaction product for 12 hours at the temperature of 60 ℃ to obtain the short-rod self-assembled spherical VOOH powder.
As can be seen from fig. 1, all diffraction peaks point to the VOOH powder, and no other miscellaneous peaks appear, so that the VOOH powder has high phase purity. Meanwhile, the rough background indicates that the VOOH powder has lower crystallinity.
As can be seen from FIG. 2, when the reaction fill ratio was increased to 70%, the synthesized product was mainly VS2And simultaneously, the production of the heterogeneous S simple substance is also accompanied. Therefore, too high a fill ratio is detrimental to the synthesis of VOOH.
As can be seen from fig. 3, when the reaction fill ratio is reduced to 50%, the synthesized product is mainly elemental sulfur, and no VOOH is synthesized. Therefore, too low a reaction fill ratio is also not favorable for the synthesis of VOOH.
As can be seen from fig. 4, the VOOH has a uniform morphology, all being in the shape of microspheres, and the microspheres are stacked on top of each other.
As can be seen from FIG. 5, the size of the microspheres is 2-5 μm, and the microspheres are self-assembled by submicron rods with the diameter of 100-500 nm and the length of 200-1000 nm.
From FIG. 6, it can be seen that the submicron rods are assembled by the nanoparticles and have a hexagonal shape, and some of the rods are crossed and some of the rods are broken.
As can be seen from fig. 7, the VOOH submicron stub has a solid structure.
As can be seen from fig. 8, the VOOH submicron short rod is self-assembled from ultra-small nanoparticles.
As can be seen from fig. 9, the diffraction fringes of VOOH have lower sharpness, indicating that the VOOH has lower crystallinity.
As can be seen in FIG. 10, the resulting product consists of VOOH nanorods and VS2The nano-sheet consists of two parts. Thus, higher NaOH concentrations will produce large amounts of VS in the synthesis product2The impure phase is not favorable for the synthesis of pure phase VOOH.
Example 2:
the method comprises the following steps: dissolving 0.8g of sodium metavanadate and 2.9g of thioacetamide in 55ml of deionized water by magnetic stirring at 500r/min for 55min to obtain a solution A;
step two: dropwise adding 0.7mol/L NaOH into the solution A under magnetic stirring, wherein the dropping speed of the NaOH solution is 0.09ml/min, dropwise adding the previous drop of the NaOH solution, stirring until the pH value of the solution is stable, and then dropwise adding the next drop of the NaOH solution until the pH value of the reaction solution is adjusted to 12.8 to obtain a solution B;
step three: transferring the solution B into a hydrothermal reaction lining according to a filling ratio of 55%, adding an outer kettle, placing the outer kettle in a homogeneous reactor, and heating the mixture from room temperature to 183 ℃ in a 7r/min rotating state to perform hydrothermal reaction for 23.5 hours;
step four: and after the hydrothermal reaction is finished and the reaction product is naturally cooled, taking out the reaction product, washing the reaction product with water and alcohol for 5 times in a centrifugal mode, centrifugally collecting the reaction product, and drying the reaction product for 13 hours at the temperature of 55 ℃ to obtain short-rod self-assembled spherical VOOH powder.
Example 3:
the method comprises the following steps: dissolving 1.1g of sodium metavanadate and 2.8g of thioacetamide in 58ml of deionized water by magnetic stirring at the speed of 400r/min for 58min to obtain a solution A;
step two: dropwise adding 0.9mol/L NaOH into the solution A under magnetic stirring, wherein the dropping speed of the NaOH solution is 0.10ml/min, after the previous drop of the NaOH solution is added, stirring until the pH value of the solution is stable, and then adding the next drop of the NaOH solution until the pH value of the reaction solution is adjusted to 13.1 to obtain a solution B;
step three: transferring the solution B into a hydrothermal reaction lining according to a filling ratio of 63 percent, adding an outer kettle, placing the outer kettle in a homogeneous phase reactor, and heating the mixture from room temperature to 185 ℃ in a rotating state of 6r/min to perform hydrothermal reaction for 23.5 hours;
step four: and after the hydrothermal reaction is finished and the reaction product is naturally cooled, taking out the reaction product, washing the reaction product for 6 times by using water and alcohol in a suction filtration washing mode, then carrying out suction filtration and collection, and drying the reaction product for 11 hours at 63 ℃ to obtain short-rod self-assembled spherical VOOH powder.
Example 4:
the method comprises the following steps: dissolving 0.9g of sodium metavanadate and 3.2g of thioacetamide in 65ml of deionized water by magnetic stirring at 450r/min for 65min to obtain a solution A;
step two: dropwise adding 0.9mol/L NaOH into the solution A under magnetic stirring, wherein the dropping speed of the NaOH solution is 0.12ml/min, after the previous drop of the NaOH solution is added, stirring until the pH value of the solution is stable, and then adding the next drop of the NaOH solution until the pH value of the reaction solution is adjusted to 12.9 to obtain a solution B;
step three: transferring the solution B into a hydrothermal reaction lining according to a filling ratio of 58%, adding an outer kettle, placing the outer kettle in a homogeneous reactor, and heating the mixture from room temperature to 175 ℃ under a rotating state of 8r/min to perform hydrothermal reaction for 24.5 hours;
step four: and after the hydrothermal reaction is finished and the reaction product is naturally cooled, taking out the reaction product, washing the reaction product with water and alcohol in a centrifugal mode for 4 times, performing suction filtration and collection, and drying the reaction product for 13 hours at the temperature of 58 ℃ to obtain short-rod self-assembled spherical VOOH powder.
Example 5:
the method comprises the following steps: dissolving 1.2g of sodium metavanadate and 3.1g of thioacetamide in 63ml of deionized water by magnetic stirring at 550r/min for 63min to obtain a solution A;
step two: dropwise adding 0.7mol/L NaOH into the solution A under magnetic stirring, wherein the dropping speed of the NaOH solution is 0.11ml/min, after the previous drop of the NaOH solution is added, stirring until the pH value of the solution is stable, and then adding the next drop of the NaOH solution until the pH value of the reaction solution is adjusted to 13.2 to obtain a solution B;
step three: transferring the solution B into a hydrothermal reaction lining according to a filling ratio of 65%, adding an outer kettle, placing the outer kettle in a homogeneous reactor, and heating the mixture from room temperature to 178 ℃ in a 6r/min rotating state to perform hydrothermal reaction for 24 hours;
step four: and after the hydrothermal reaction is finished and the reaction product is naturally cooled, taking out the reaction product, washing the reaction product by water and alcohol for 5 times in a suction filtration washing mode, centrifugally collecting the reaction product, and drying the reaction product for 11 hours at the temperature of 65 ℃ to obtain the short-rod self-assembled spherical VOOH powder.

Claims (7)

1. A preparation method of short-rod self-assembled spherical VOOH powder is characterized by comprising the following steps:
the method comprises the following steps: dissolving 0.8-1.2 g of sodium metavanadate and 2.8-3.2 g of thioacetamide in 55-65 ml of deionized water under magnetic stirring to obtain a solution A;
step two: dropwise adding 0.7-0.9 mol/L NaOH solution into the solution A under magnetic stirring to adjust the pH value of the solution A to 12.8-13.2, and obtaining solution B;
step three: transferring the solution B into a hydrothermal reaction lining, adding an outer kettle, placing the outer kettle into a homogeneous phase reactor, and heating the solution B to 175-185 ℃ from room temperature under a rotating state to perform hydrothermal reaction;
step four: after the hydrothermal reaction is finished and the reaction product is naturally cooled, taking out the reaction product, washing with water and alcohol, collecting the reaction product, and drying the reaction product at the temperature of 55-65 ℃ to obtain short-rod self-assembled spherical VOOH powder;
the dropping speed of the NaOH solution in the second step is 0.08-0.12 ml/min, the previous drop of NaOH solution is dropped, the solution is stirred until the pH value of the solution is stable, and then the next drop of NaOH solution is dropped until the pH value of the reaction solution is adjusted to 12.8-13.2;
the filling ratio of the solution B transferred to the hydrothermal reaction lining in the third step is 55-65%;
the VOOH powder has a uniform three-stage self-assembly structure, and is formed by self-assembling ultra-small nano particles into submicron short rods, wherein the submicron short rods are self-assembled into micron balls, the diameter of each VOOH short rod is 100-500 nm, the length of each VOOH short rod is 200-1000 nm, each VOOH short rod is formed by assembling nano small particles, each VOOH short rod is hexagonal, part of the VOOH short rods are crossed, part of the VOOH short rods are broken, and the diameter of each VOOH ball formed by self-assembling the short rods is 2-5 mu m.
2. The method for preparing a short-rod self-assembled spherical VOOH powder according to claim 1, wherein the method comprises the following steps: the rotating speed of the magnetic stirring in the first step is 400-600 r/min, and the stirring time is 55-65 min.
3. The method for preparing a short-rod self-assembled spherical VOOH powder according to claim 1, wherein the method comprises the following steps: the rotation speed of the hydrothermal reaction in the third step is 5-8 r/min.
4. The method for preparing a short-rod self-assembled spherical VOOH powder according to claim 1, wherein the method comprises the following steps: the hydrothermal reaction time of the third step is 23.5-24.5 h.
5. The method for preparing a short-rod self-assembled spherical VOOH powder according to claim 1, wherein the method comprises the following steps: and step four, washing with water, washing with alcohol by adopting suction filtration washing or centrifugal washing for 3-6 times respectively, and collecting by adopting suction filtration collection or centrifugal collection.
6. The method for preparing a short-rod self-assembled spherical VOOH powder according to claim 1, wherein the method comprises the following steps: and the drying time of the fourth step is 11-13 h.
7. An application of the short self-assembled spherical VOOH powder of claim 6 in the fields of sodium/lithium/magnesium ion batteries, supercapacitors and photo/electrocatalysis.
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