CN108163891B - Three-dimensional self-assembly NaV2O5Micron powder and preparation method and application thereof - Google Patents
Three-dimensional self-assembly NaV2O5Micron powder and preparation method and application thereof Download PDFInfo
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Abstract
Three-dimensional self-assemblyContaining NaV2O5Micron powder of sodium metavanadate and Na, its preparation and application2S·9H2Adding O into deionized water to obtain a solution A; pouring the solution A into a reaction inner liner, sealing, placing the inner liner in an outer kettle, fixing, and placing in a homogeneous phase reactor for hydrothermal reaction; collecting a product after the hydrothermal reaction is finished, and alternately cleaning the product by water and alcohol; putting the collected product into a cold well of a freeze dryer for freezing and carrying out vacuum-pumping drying to obtain the three-dimensional self-assembled NaV2O5Micron powder. Three-dimensional self-assembly NaV2O5The micron powder body is composed of micron beams with the diameter of 5-10 microns, the micron beams are formed by self-assembling submicron rods with the diameter of 200nm, and the submicron rods are of a mesomorphic structure. When the material is applied to the negative electrode of the lithium ion battery, the material returns to 100mAg after being subjected to a large rate test‑1At a current density of 291mAhg, the capacity was still maintained‑1At 100mAg‑1The current density of the capacitor is increased, the capacitor circulates for 360 circles, and the capacity reaches 580mAhg‑1NaV during the test of multiplying power and cycle performance2O5The micron powder shows stable coulombic efficiency.
Description
Technical Field
The invention relates to a NaV2O5Powder and a preparation method thereof, in particular to three-dimensional self-assembly NaV2O5Micron powder and its preparation process and application.
Background
NaV2O5The vanadium-oxygen composite material is considered to be an energy storage material with great development prospect due to the unique vanadium-oxygen framework, the stable structure, the larger interlayer spacing, the excellent physical and chemical properties and the existence of a large number of oxygen vacanciesThe material is applied to the field of positive electrodes of sodium-ion batteries [ Liu P, Zhou D, Zhu K, Wu Q, Wang Y, Tai G, et al2O5mesocrystals:from synthesis,growth mechanism to analysis ofNa-ion intercalation/deintercalation abilities.Nanoscale. 2016；8:1975-85.]However, there is no report on its application as a negative electrode material of a lithium ion battery. In addition, previously with respect to NaV2O5There are two main reports of the synthesis method (2). One is a solid phase method, which has high synthesis temperature, complex reaction, large energy consumption and high cost. The other is a two-step hydrothermal method, and although the synthesis temperature is low, the synthesis process is long and complicated.
Disclosure of Invention
The invention aims to provide a three-dimensional self-assembled NaV2O5Micron powder and its preparation process and application.
In order to achieve the purpose, the preparation method comprises the following steps:
the method comprises the following steps: taking 0.8-1.2 g of sodium metavanadate and 0.05-0.1 g of Na2S·9H2Adding O into 55-65 ml of deionized water, and magnetically stirring or ultrasonically dispersing to obtain a semi-clear solution A;
step two: pouring the solution A into a reaction inner liner according to a filling ratio of 55-65%, sealing, placing the inner liner in an outer kettle, fixing, placing in a homogeneous reactor, and heating from room temperature to 195-205 ℃ under the condition of a rotating speed of 5-15 r/min to perform hydrothermal reaction;
step three: after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, collecting a product, and alternately cleaning the product for 3-6 times by using water and alcohol;
step four: placing the collected product in a cold well of a freeze dryer for freezing, then placing the frozen product in a tray, covering a sealing cover, vacuumizing to 10-20 Pa, drying for 12-18 h, and collecting the product to obtain the three-dimensional self-assembled NaV2O5Micron powder.
The magnetic stirring or ultrasonic treatment time in the first step is 55-65 min, and the rotating speed of the magnetic stirring is 800-1000 r/min.
And the hydrothermal reaction time of the second step is 23-25 h.
And collecting in the third step by suction filtration or centrifugation.
And the cleaning in the third step is carried out by suction filtration or centrifugation.
The refrigeration conditions of the step four are as follows: freezing for 2-5 hours at-60 to-40 ℃.
And sealing the product obtained in the step four by using a preservative film before the product is placed into a tray for drying, and pricking holes on the preservative film to ensure that the product is sufficiently dried under a low-pressure condition.
Three-dimensional self-assembled NaV prepared by the preparation method of the invention2O5The micron powder body is composed of micron beams with the diameter of 5-10 microns, the micron beams are formed by self-assembling submicron rods with the diameter of 200nm, and the submicron rods are of a mesomorphic structure.
The three-dimensional self-assembly NaV of the invention2O5When the micron powder is applied to the negative electrode of a lithium ion battery, the concentration is 100, 200, 500, 1000 and 2000mAg-1The capacity can reach 259, 232, 192, 151 and 115mAhg respectively at the current density of (1)-1After undergoing a large magnification test, return to 100mAg-1At a current density of 291mAhg, the capacity was still maintained-1At 100mAg-1The current density of the capacitor is increased, the capacitor circulates for 360 circles, and the capacity reaches 580mAhg-1NaV during the test of multiplying power and cycle performance2O5The micron powder shows stable coulombic efficiency.
The invention adopts an extremely simple and efficient one-step low-temperature hydrothermal method to synthesize high-purity three-dimensional self-assembled NaV2O5The method has the advantages of simple and easily-controlled reaction process, low temperature, high yield of synthetic products and no need of large-scale equipment and harsh reaction conditions. When the product is applied to a lithium ion battery cathode material, excellent rate and cycle performance are shown.
The concrete expression is as follows:
1) the invention adopts one-step hydrothermal reaction to directly synthesize the final product, thereby having low synthesis temperature and not needing large-scale equipment and harsh reaction conditions;
2) the invention makes full use of trace Na2S·9H2S provided after O is dissolved in water2-Reducing ions, and adding NaVO as raw material3Directly reduce to NaV2O5Therefore, the method has the advantages of simple synthesis path, easy control of reaction, high yield, no need of post-treatment, environmental friendliness and suitability for large-scale production;
3) the raw materials used by the invention are sodium metavanadate and Na2S·9H2O, deionized water is adopted as a solvent, and the solvents are common substances, are cheap and easy to obtain and have low cost;
4) the invention needs to strictly control Na2S·9H2The addition of O, too little of which could not add NaVO3Fully reduced to NaV2O5Excessive addition will produce a nanosheet structure. Thus, Na2S·9H2Addition of O to three-dimensional self-assembled NaV2O5The synthesis of micron powder plays a very critical role;
5) the invention also needs to strictly control the reaction temperature, and the excessively low reaction temperature is not beneficial to three-dimensional self-assembly of NaV2O5Generating micron powder;
6) in the process of synthesizing the three-dimensional self-assembly structure, no template agent or surfactant is introduced, and the whole self-assembly process is controlled by topological transformation of reaction raw materials, so that the whole reaction is simple, easy to control, high-efficiency and low in cost;
7) NaV prepared by the invention2O5A large number of oxygen vacancies exist on the surface, so that a large number of active sites are provided for the storage and rapid transmission of lithium ions;
8) the invention prepares three-dimensional self-assembly NaV2O5The micron powder has a unique three-dimensional structure formed by self-assembly of submicron rods. The self-assembly structure with the submicron rods in mutual contact can play a good role in physical confinement on one hand, and also provides a buffer space for the expansion and contraction of the submicron rods on the other hand, so that the volume change of the submicron rods can be greatly relieved, and the circulation of the submicron rods is finally obviously improvedStability;
9) the invention prepares three-dimensional self-assembly NaV2O5The submicron rod of the structure in the micron powder body has smaller scale, not only can generate larger specific surface area, but also can provide more surface active sites, thereby improving the electrochemical performance. In addition, the ultra-small scale can not only shorten a charge transfer path, but also provide more active sites for the storage of lithium ions, thereby improving the specific capacity and rate capability of the material;
10) the invention prepares three-dimensional self-assembly NaV2O5Submicron rod NaV of structure in micron powder2O5The mesoporous crystal has mesoscopic crystal characteristics of oriented growth along a (001) crystal plane, and the larger interplanar spacing of the mesoporous crystal can provide better space for rapid and sufficient occurrence of electrochemical reaction. At the same time, NaV2O5The mesoscopic crystal has single crystal characteristics and high crystallinity, so that the mesoscopic crystal can show excellent structural stability in the charge and discharge processes;
11) the product prepared by the method has the advantages of uniform chemical composition, high purity and uniform appearance, and can show excellent electrochemical performance when being used as a lithium ion battery cathode material. In the voltage range of 0.01-3.0, 100, 200, 500, 1000 and 2000mAg-1Shows as high as 259, 232, 192, 151 and 115mAhg at current density of (A)-1When the specific capacity of the resin is returned to 100mAg-1The capacity can reach 291mAhg at the current density of-1. At 100mAg-1The capacity can reach 580mAhg after 360 circles of circulation under the current density of-1. In addition, stable coulombic efficiency is shown in the whole test process of multiplying power and cycle performance.
Drawings
FIG. 1 is an X-ray diffraction pattern of the product prepared in example 1 of this invention.
FIG. 2 is a scanning electron microscope image of sodium metavanadate as a raw material used in the present invention.
FIG. 3 is a scanning electron micrograph of a product prepared according to example 1 of the present invention.
FIG. 4 is a high power SEM image of the product of example 1 of the present invention.
FIG. 5 is an ultra-high magnification SEM image of a product prepared in example 1 of the present invention.
FIG. 6 is a transmission electron micrograph of a product prepared in example 1 of the present invention.
FIG. 7 is a diffraction pattern of a product prepared in example 1 of the present invention.
Fig. 8 is a graph of rate capability of the product prepared in example 1 of the present invention as a negative electrode of a lithium ion battery.
Fig. 9 shows the cycle performance of the product prepared in example 1 of the present invention as a negative electrode material of a lithium ion battery.
FIG. 10 shows Na in example 1 of the present invention2S·9H2When the addition amount of O is increased to 0.5g, the structure of the synthesized product is a nanosheet structure.
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: taking 1.0g of sodium metavanadate and 0.08g of Na2S·9H2Adding O into 60ml deionized water, and magnetically stirring at 800r/min for 65min to obtain a semi-clear solution A;
step two: pouring the solution A into a reaction lining according to the filling ratio of 60%, sealing, placing the lining in an outer kettle, fixing, placing in a homogeneous reactor, and heating from room temperature to 200 ℃ at the rotation speed of 10r/min to perform hydrothermal reaction for 24 hours;
step three: naturally cooling the reaction kettle to room temperature after the hydrothermal reaction is finished, collecting a product by adopting suction filtration, and alternately cleaning the product by adopting suction filtration for 3 times through water and alcohol;
step four: placing the collected product in a cold well of a freeze dryer, freezing for 2 hours at-60 ℃, then placing the frozen product in a tray, covering a sealing cover, vacuumizing to 15Pa, drying for 12 hours, and collecting the product to obtain the three-dimensional self-assembled NaV2O5Micron powder.
From FIG. 1, it can be clearly seen that the diffraction peak of the synthesized product and the NaV of the orthorhombic phase2O5The standard card PDF #89-8040 is completely matched, and the synthesized product is pure-phase orthorhombic phase NaV2O5. In addition, the smooth and slender diffraction peak shows that the product has good crystallinity, and the intensity of the diffraction peak corresponding to the (001) crystal face is strongest, which indicates that the product has the characteristic of remarkable oriented growth along the (001) crystal face.
As can be seen from fig. 2, the sodium metavanadate source is composed of self-assembled micro-beams of sub-rods.
As can be seen from FIG. 3, the obtained product exhibits a microstructure similar to that of the sodium metavanadate raw material, i.e., the product is self-assembled into a 5-10 μm micron beam by uniform submicron rods.
As can be clearly seen in fig. 4, the sub-micron rods are tightly packed together to form a micro-beam.
As is clear from FIG. 5, the submicron rods have a diameter of about 200nm and have a large aspect ratio.
From FIG. 6, it can be further seen that the submicron rods are micro-solid structures and have a diameter of about 200 nm.
It can be seen from fig. 7 that the submicron rods exhibit a clear single crystal structure.
As can be seen in FIG. 8, at 100, 200, 500, 1000 and 2000mAg-1The capacity can reach 259, 232, 192, 151 and 115mAhg respectively at the current density of (1)-1After undergoing a large rate test, return to 100mAg-1At a current density of 291mAhg, the capacity was still able to be reached-1. Meanwhile, under the condition of different multiplying powers, the product shows excellent coulombic efficiency,
as can be seen from FIG. 9, at 100mAg-1The current density of the capacitor is circulated for 360 circles, and the capacity can reach 580mAhg-1. Meanwhile, the whole circulation process shows stable coulombic efficiency.
FIG. 10 shows Na in example 1 of the present invention2S·9H2When the addition amount of O is increased to 0.5g, the structure of the synthesized product is a nanosheet structure. It is worth mentioning that Na is not added when2S·9H2And when O is in the range, the hydrothermal reaction is finished to obtain a clear solution, and no precipitate is generated. When the reaction temperature in example 1 of the present invention was decreased to 180 ℃, the hydrothermal reaction was followed by a clear solution without precipitationAnd (4) generating the substance. Therefore, too little Na2S·9H2Both the addition of O and the excessively low reaction temperature are detrimental to NaV2O5And (4) synthesizing.
Example 2:
the method comprises the following steps: taking 0.8g of sodium metavanadate and 0.05g of Na2S·9H2Adding O into 55ml deionized water, and magnetically stirring at 900r/min for 60min to obtain semi-clear solution A;
step two: pouring the solution A into a reaction lining according to a filling ratio of 58%, sealing, placing the lining in an outer kettle, fixing, placing in a homogeneous reactor, and heating from room temperature to 195 ℃ under the condition of a rotating speed of 8r/min to perform hydrothermal reaction for 25 hours;
step three: after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, collecting a product by centrifugation, and alternately cleaning the product by water and alcohol for 5 times by centrifugation;
step four: placing the collected product in a cold well of a freeze dryer at-55 ℃, freezing for 3 hours, then placing the frozen product in a tray, sealing the tray by using a preservative film, puncturing the preservative film, covering a sealing cover, vacuumizing to 12Pa, drying for 15 hours, and collecting the product to obtain the three-dimensional self-assembled NaV2O5Micron powder.
Example 3:
the method comprises the following steps: taking 1.2g of sodium metavanadate and 0.06g of Na2S·9H2Adding O into 65ml deionized water, and magnetically stirring for 55min at 1000r/min to obtain a semi-clear solution A;
step two: pouring the solution A into a reaction lining according to a filling ratio of 65%, sealing, placing the lining in an outer kettle, fixing, placing in a homogeneous reactor, and heating from room temperature to 205 ℃ at a rotating speed of 12r/min to perform hydrothermal reaction for 23 h;
step three: after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, collecting a product by adopting suction filtration, and alternately cleaning the product by water and alcohol for 4 times by adopting centrifugation;
step four: placing the collected product in a cold well of a freeze dryer at-45 deg.C, freezing for 4 hr, placing the frozen product in a tray, sealing with a preservative film, and sealingPricking holes on the preservative film, covering a sealing cover, vacuumizing to 18Pa, drying for 18h, and collecting a product to obtain the three-dimensional self-assembled NaV2O5Micron powder.
Example 4:
the method comprises the following steps: taking 0.9g of sodium metavanadate and 0.07g of Na2S·9H2Adding O into 58ml of deionized water, and performing ultrasonic dispersion for 58min to obtain a semi-clear solution A;
step two: pouring the solution A into a reaction inner liner according to a filling ratio of 55%, sealing, placing the inner liner in an outer kettle, fixing, placing in a homogeneous phase reactor, and heating from room temperature to 198 ℃ under the condition of a rotating speed of 5r/min to perform hydrothermal reaction for 25 hours;
step three: after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, collecting a product by centrifugation, and alternately cleaning the product by water and alcohol by suction filtration for 6 times;
step four: placing the collected product in a cold well of a freeze dryer at-40 ℃, freezing for 5 hours, then placing the frozen product in a tray, sealing the tray by using a preservative film, puncturing the preservative film, covering a sealing cover, vacuumizing to 10Pa, drying for 16 hours, and collecting the product to obtain the three-dimensional self-assembled NaV2O5Micron powder.
Example 5:
the method comprises the following steps: taking 1.1g of sodium metavanadate and 0.1g of Na2S·9H2Adding O into 62ml of deionized water, and performing ultrasonic dispersion for 63min to obtain a semi-clear solution A;
step two: pouring the solution A into a reaction lining according to the filling ratio of 62%, sealing, placing the lining in an outer kettle, fixing, placing in a homogeneous reactor, and heating from room temperature to 202 ℃ at the rotation speed of 15r/min to perform hydrothermal reaction for 24 hours;
step three: after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, collecting a product by centrifugation, and alternately cleaning the product by water and alcohol for 5 times by centrifugation;
step four: placing the collected product in a cold well of a freeze dryer at-50 deg.C, freezing for 4 hr, placing the frozen product in a tray, sealing with a preservative film, and packaging with the preservative filmPricking holes, covering a sealing cover, vacuumizing to 20Pa, drying for 13h, and collecting a product to obtain the three-dimensional self-assembled NaV2O5Micron powder.
Claims (7)
1. Three-dimensional self-assembly NaV2O5The preparation method of the micron powder is characterized by comprising the following steps:
the method comprises the following steps: taking 0.8-1.2 g of sodium metavanadate and 0.05-0.1 g of Na2S·9H2Adding O into 55-65 ml of deionized water, and magnetically stirring or ultrasonically dispersing to obtain a semi-clear solution A;
step two: pouring the solution A into a reaction inner liner according to a filling ratio of 55-65%, sealing, placing the inner liner in an outer kettle, fixing, placing in a homogeneous reactor, and heating from room temperature to 195-205 ℃ under the condition of a rotating speed of 5-15 r/min to perform hydrothermal reaction;
step three: after the hydrothermal reaction is finished, naturally cooling the reaction kettle to room temperature, collecting a product, and alternately cleaning the product for 3-6 times by using water and alcohol;
step four: placing the collected product in a cold well of a freeze dryer for freezing, then placing the frozen product in a tray, covering a sealing cover, vacuumizing to 10-20 Pa, drying for 12-18 h, and collecting the product to obtain the three-dimensional self-assembled NaV2O5Micron powder;
and the hydrothermal reaction time of the second step is 23-25 h.
2. The three-dimensional self-assembling NaV of claim 12O5The preparation method of the micron powder is characterized by comprising the following steps: the magnetic stirring or ultrasonic treatment time in the first step is 55-65 min, and the rotating speed of the magnetic stirring is 800-1000 r/min.
3. The three-dimensional self-assembling NaV of claim 12O5The preparation method of the micron powder is characterized by comprising the following steps: and collecting in the third step by suction filtration or centrifugation.
4. The three-dimensional self-assembling NaV of claim 12O5The preparation method of the micron powder is characterized by comprising the following steps: and the cleaning in the third step is carried out by suction filtration or centrifugation.
5. The three-dimensional self-assembling NaV of claim 12O5The preparation method of the micron powder is characterized by comprising the following steps: the refrigeration conditions of the step four are as follows: freezing for 2-5 hours at-60 to-40 ℃.
6. The three-dimensional self-assembling NaV of claim 12O5The preparation method of the micron powder is characterized by comprising the following steps: and sealing the product obtained in the step four by using a preservative film before the product is placed into a tray for drying, and pricking holes on the preservative film to ensure that the product is sufficiently dried under a low-pressure condition.
7. A three-dimensional self-assembled NaV prepared by the method of claim 12O5The application of the micron powder is 100, 200, 500, 1000 and 2000mAg when the micron powder is applied to a lithium ion battery cathode-1The capacity can reach 259, 232, 192, 151 and 115mAhg respectively at the current density of (1)-1After undergoing a large magnification test, return to 100mAg-1At a current density of 291mAhg, the capacity was still maintained-1At 100mAg-1The current density of the capacitor is increased, the capacitor circulates for 360 circles, and the capacity reaches 580mAhg-1NaV during the test of multiplying power and cycle performance2O5The micron powder shows stable coulombic efficiency.
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