CN109264781B - Cd2V2O7Nano material, preparation method thereof and Cd2V2O7Composite electrode - Google Patents
Cd2V2O7Nano material, preparation method thereof and Cd2V2O7Composite electrode Download PDFInfo
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Abstract
The invention discloses a Cd2V2O7The preparation method of the nano material comprises the steps of preparing cadmium salt and vanadium pentoxide by a one-step hydrothermal method, wherein the material is a vanadium-cadmium bimetallic oxide and is of a two-dimensional nanosheet structure, so that the material is beneficial to shortening of an ion transmission path, improvement of electronic conductivity and embedding and extraction of lithium ions, the rate capability and specific capacity of the material are improved, the conductivity and specific capacity of the material can be improved, and Cd prepared by the material2V2O7The composite electrode has high specific capacity and good cycling stability, and improves the electrochemical performance of the material.
Description
Technical Field
The invention relates to the field of new energy materials, in particular to Cd2V2O7A nano material and a preparation method thereof, and also relates to a Cd2V2O7And (3) a composite electrode.
Background
The consumption of fossil energy brings a series of environmental pollution problems, and the development of novel clean energy is a technical problem to be solved urgently at present. Typical green energy storage devices such as lithium ion batteries and super capacitors, especially lithium ion batteries, have the advantages of high specific capacity, wide voltage range, large energy density, etc., are developed very rapidly, and have already been commercialized.
The electrochemical performance of lithium ion batteries depends to a large extent on the intrinsic properties, structure and morphology of the electrode material. At present, the commercial lithium ion battery cathode material is mainly a graphite electrode which has good conductivity, but the further application of the lithium ion battery cathode material in the lithium ion battery is restricted due to the poor energy density and volume density of the lithium ion battery cathode material. Transition metal vanadium and oxides thereof have been the electrode materials of great interest to scientists. With vanadium (V) pentoxide2O5) For example, vanadium exists in multiple valence states from +3 to +5, intercalation at multiple positions can occur, and V2O5The unique layered structure facilitates the de-intercalation of ions, thus V2O5The theoretical capacity of the composite material can reach 442mAh/g at most. The electrochemical performance of vanadium oxide is inherently good, but still has the following defects: the vanadium oxide material of the block body has low conductivity and small lithium ion diffusion coefficient, so that the specific capacity is low and the rate capability is poor. Due to these inherent drawbacks, their use is limited.
Disclosure of Invention
Aiming at the defects, the invention provides Cd2V2O7The preparation method of the nano material is simple, the raw materials are easy to obtain, the cost is low, and the Cd prepared by the preparation method2V2O7Cd prepared from nano material2V2O7The composite electrode has good specific capacity and stability.
In order to achieve the purpose, the invention adopts the following technical scheme:
cd (cadmium)2V2O7The preparation method of the nano material comprises the following steps:
a. adding cadmium salt and vanadium pentoxide into deionized water, and uniformly stirring to form a solution a;
b. adding ammonia water into the solution a while stirring, and then continuously stirring to form a solution b;
c. transferring the solution b to a hydrothermal reaction kettle for hydrothermal reaction to obtain a product;
d. cooling the product, separating, washing and drying to obtain Cd2V2O7And (3) nano materials.
Preferably, the cadmium salt is cadmium sulfate or cadmium nitrate, the purpose of which is to provide a cadmium source, the ionic cadmium source being more favorable for the reaction to occur.
Further, in the step a, the amount of the cadmium salt is 0.5-1.5 mmol, the amount of the vanadium pentoxide is 1-2 mmol, the amount of the deionized water is 25-35 ml, and the stirring time is 20-40 min, wherein the stirring may be magnetic stirring or mechanical stirring, and the main purpose is to completely dissolve the cadmium salt and the vanadium pentoxide in the deionized water and form a uniform solution a, and in the embodiment of the present invention, the magnetic stirring is preferred.
Further, in the step b, the using amount of the ammonia water is 5-10 ml, the continuous stirring time is 5-15 min, on one hand, the adding of the ammonia water provides a weak alkaline atmosphere, and on the other hand, ammonium ions have complexation and are beneficial to forming nanosheets.
Further, in the step c, the hydrothermal reaction is carried out for 10-16 hours at 140-180 ℃.
Further, in step d, the separation is centrifugal separation, the washing comprises deionized water washing and absolute ethyl alcohol washing, mainly for washing away residues on the surface of the product and purifying the product, wherein the preferred washing process is that the deionized water washing and the absolute ethyl alcohol washing are alternately carried out in sequence, and at least one washing is alternately carried out. The drying is vacuum drying at 90-100 ℃.
The invention also aims to provide Cd prepared by the preparation method2V2O7And (3) nano materials.
The third purpose of the invention is to provide a method for using the Cd2V2O7Cd prepared from nano material2V2O7Composite electrode, Cd in the invention2V2O7The preparation method of the composite electrode is a conventional electrode preparation method in the field, and the composite electrode is prepared by adopting the following method in the embodiment of the invention: the Cd prepared above is2V2O7The nano material is used as an active substance of the negative electrode, and is fully mixed with carbon black and a polyvinylidene fluoride N-methyl pyrrolidone solution with the mass concentration of 5% under stirring to prepare uniform slurry which is used as a composite negative electrode material for later use. The slurry comprises the following components in percentage by mass: cd [ Cd ]2V2O780-90% of nano material, 5-10% of carbon black and 5-10% of polyvinylidene fluoride. Uniformly coating the slurry on a current collector copper foil, drying and rolling to obtain Cd2V2O7And (3) a composite electrode.
Compared with the prior art, the invention has the following beneficial effects:
successfully preparing Cd by a one-step hydrothermal method2V2O7The nano material is a vanadium and cadmium bimetal oxide, can improve the conductivity and specific capacity of the material, and the Cd is2V2O7The nano material is of a nano flaky structure, which is beneficial to shortening of an ion transmission path and improvement of electronic conductivity, and is beneficial to insertion and extraction of lithium ions, so that the rate capability and specific capacity of the material are improved, and thus the Cd prepared from the material2V2O7The composite electrode has high specific capacity and good cycling stability, and improves the electrochemical performance of the material.
Drawings
FIG. 1 shows Cd in example 1 of the present invention2V2O7Scanning electron microscopy of the nanomaterial;
FIG. 2 shows Cd in example 1 of the present invention2V2O7XRD pattern of the nano material;
FIG. 3 shows Cd in example 1 of the present invention2V2O7Constant current charge and discharge test chart of the composite electrode;
FIG. 4 shows Cd in example 1 of the present invention2V2O7Cyclic material test pattern of composite electrodes.
Detailed Description
The invention is further illustrated below with reference to specific examples. The following examples are provided only for explaining and illustrating the present invention and are not to be construed as limiting the scope of the present invention. The test methods in the following examples, in which specific conditions are not specified, are generally conventional conditions or conditions recommended by the manufacturer.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
Dissolving 0.5mmol of cadmium sulfate and 1mmol of vanadium pentoxide in 25mL of ionic water, and magnetically stirring for 30min to form a uniform solution a; then, stirring the mixtureAdding 5mL of ammonia water into the solution a to form a uniform solution b; then transferring the solution b to a hydrothermal reaction kettle for sealing at 160 DEGoCarrying out hydrothermal reaction for 10 hours at the temperature of C to obtain a product; cooling the product, performing centrifugal separation, sequentially and alternately washing for 3 times by using deionized water and absolute ethyl alcohol, and then performing vacuum drying on the washed product at 90 ℃ to obtain Cd2V2O7And (3) nano materials.
The obtained Cd is2V2O7The nano material is used as a negative electrode active substance, and is fully stirred and mixed with carbon black and a polyvinylidene fluoride N-methyl pyrrolidone solution with the mass concentration of 5% to prepare uniform slurry which is used as a composite negative electrode material for later use. The slurry comprises the following components in percentage by mass: cd [ Cd ]2V2O780% of nano material, 10% of carbon black and 10% of polyvinylidene fluoride. Uniformly coating the slurry on a current collector copper foil, drying and rolling to obtain Cd2V2O7And (3) a composite electrode.
Example 2
Dissolving 1mmol of cadmium nitrate and 1.5mmol of vanadium pentoxide in 30mL of ionic water, and magnetically stirring for 30min to form a uniform solution a; then, adding 7mL of ammonia water into the solution a while stirring to form a uniform solution b; then transferring the solution b to a hydrothermal reaction kettle, sealing and performing 150 ℃ reactionoCarrying out hydrothermal reaction for 12 hours at the temperature of C to obtain a product; cooling the product, performing centrifugal separation, sequentially and alternately washing for 3 times by using deionized water and absolute ethyl alcohol, and then performing vacuum drying on the washed product at 90 ℃ to obtain Cd2V2O7And (3) nano materials.
The obtained Cd is2V2O7The nano material is used as a negative electrode active substance, and is fully stirred and mixed with carbon black and a polyvinylidene fluoride N-methyl pyrrolidone solution with the mass concentration of 5% to prepare uniform slurry which is used as a composite negative electrode material for later use. The slurry comprises the following components in percentage by mass: cd [ Cd ]2V2O785% of nano material, 10% of carbon black and 5% of polyvinylidene fluoride. Uniformly coating the slurry on a current collector copper foil, drying and rolling to obtain Cd2V2O7And (3) a composite electrode.
Example 3
Dissolving 1.5mmol of cadmium sulfate and 2mmol of vanadium pentoxide in 35mL of ionic water, and magnetically stirring for 30min to form a uniform solution a; then, adding 10mL of ammonia water into the solution a while stirring to form a uniform solution b; then transferring the solution b to a hydrothermal reaction kettle for sealing, and 170oCarrying out hydrothermal reaction for 14h at the temperature of C to obtain a product; cooling the product, performing centrifugal separation, sequentially and alternately washing for 3 times by using deionized water and absolute ethyl alcohol, and then performing vacuum drying on the washed product at 95 ℃ to obtain Cd2V2O7And (3) nano materials.
The obtained Cd is2V2O7The nano material is used as a negative electrode active substance, and is fully stirred and mixed with carbon black and a polyvinylidene fluoride N-methyl pyrrolidone solution with the mass concentration of 5% to prepare uniform slurry which is used as a composite negative electrode material for later use. The slurry comprises the following components in percentage by mass: cd [ Cd ]2V2O790% of nano material, 5% of carbon black and 5% of polyvinylidene fluoride. Uniformly coating the slurry on a current collector copper foil, drying and rolling to obtain Cd2V2O7And (3) a composite electrode.
Example 4
Dissolving 1mmol of cadmium sulfate and 1.5mmol of vanadium pentoxide in 30mL of ionic water, and magnetically stirring for 30min to form a uniform solution a; then, adding 10mL of ammonia water into the solution a while stirring to form a uniform solution b; then transferring the solution b to a hydrothermal reaction kettle for sealing at 140oCarrying out hydrothermal reaction for 16h at the temperature of C to obtain a product; cooling the product, performing centrifugal separation, sequentially and alternately washing for 3 times by using deionized water and absolute ethyl alcohol, and then performing vacuum drying on the washed product at 100 ℃ to obtain Cd2V2O7And (3) nano materials.
The obtained Cd is2V2O7The nano material is used as a negative electrode active substance, and is fully stirred and mixed with carbon black and a polyvinylidene fluoride N-methyl pyrrolidone solution with the mass concentration of 5 percent to be uniformThe slurry is used as a composite negative electrode material for standby. The slurry comprises the following components in percentage by mass: cd [ Cd ]2V2O785% of nano material, 5% of carbon black and 10% of polyvinylidene fluoride. Uniformly coating the slurry on a current collector copper foil, drying and rolling to obtain Cd2V2O7And (3) a composite electrode.
Example 5
Dissolving 1.5mmol of cadmium sulfate and 2mmol of vanadium pentoxide in 35mL of ionic water, and magnetically stirring for 30min to form a uniform solution a; then, adding 10mL of ammonia water into the solution a while stirring to form a uniform solution b; then transferring the solution b to a hydrothermal reaction kettle, sealing and carrying out 180 DEG CoCarrying out hydrothermal reaction for 10 hours at the temperature of C to obtain a product; cooling the product, performing centrifugal separation, sequentially and alternately washing for 3 times by using deionized water and absolute ethyl alcohol, and then performing vacuum drying on the washed product at 100 ℃ to obtain Cd2V2O7And (3) nano materials.
The obtained Cd is2V2O7The nano material is used as a negative electrode active substance, and is fully stirred and mixed with carbon black and a polyvinylidene fluoride N-methyl pyrrolidone solution with the mass concentration of 5% to prepare uniform slurry which is used as a composite negative electrode material for later use. The slurry comprises the following components in percentage by mass: cd [ Cd ]2V2O785% of nano material, 10% of carbon black and 5% of polyvinylidene fluoride. Uniformly coating the slurry on a current collector copper foil, drying and rolling to obtain Cd2V2O7And (3) a composite electrode.
The Cd prepared in example 12V2O7The nano material is characterized by a scanning electron microscope and X-ray diffraction, and the characterization result is shown in FIG. 1 and FIG. 2.
As is clear from FIG. 1, Cd obtained in example 12V2O7The nano material is of a sheet structure and has good dispersibility, and the two-dimensional sheet nano structure is beneficial to shortening an ion transmission path, improving electronic conductivity and being beneficial to the insertion and extraction of lithium ions, so that the rate capability and specific capacity of the material are improved. Will carry outCd obtained in example 12V2O7The comparison of the nanomaterial with the standard card shows that the result is shown in FIG. 2, and the characteristic peaks can be observed to be matched, which indicates that Cd is prepared in the embodiment2V2O7And (3) nano materials.
The Cd prepared in example 1 was also subjected to2V2O7The composite electrode is subjected to constant current charge and discharge and cyclic material test, the current density of the constant current charge and discharge test is 0.2A/g, the three-time charge and discharge test result is shown in figure 3, and the second charge and discharge result is relatively overlapped with the third result, which accords with the characteristics of the lithium ion battery, because the first charge and discharge can form an SEI film, partial lithium ions are consumed, and the subsequent capacity is reduced.
The test of the circulating material is to circulate 110 times under the current density of 0.2A/g to obtain a cycle time-specific capacity curve of the tested electrode, the test result is shown in figure 4, the specific capacity is reduced due to the formation of an SEI film in the initial stage of circulation, and the specific capacity is slowly improved in the later stage of circulation due to Cd2V2O7The lithium storage mechanism of the composite electrode is enhanced.
According to the test results, the Cd is successfully prepared by a one-step hydrothermal method2V2O7The nano material is a vanadium and cadmium bimetal oxide, can improve the conductivity and specific capacity of the material, and the Cd is2V2O7The nano material is of a nano flaky structure, which is beneficial to shortening of an ion transmission path and improvement of electronic conductivity, and is beneficial to insertion and extraction of lithium ions, so that the rate capability and specific capacity of the material are improved, and thus the Cd prepared from the material2V2O7The composite electrode has high specific capacity and good cycling stability, and improves the electrochemical performance of the material.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the present invention.
Claims (4)
1. Cd (cadmium)2V2O7The preparation method of the nano material is characterized by comprising the following steps: the method comprises the following steps:
a. adding cadmium salt and vanadium pentoxide into deionized water, and uniformly stirring to form a solution a, wherein the cadmium salt is cadmium sulfate or cadmium nitrate, the dosage of the cadmium salt is 0.5-1.5 mmol, the dosage of the vanadium pentoxide is 1-2 mmol, the dosage of the deionized water is 25-35 ml, and the stirring time is 20-40 min;
b. adding 5-10 ml of ammonia water into the solution a while stirring, and then continuously stirring for 5-15 min to form a solution b;
c. transferring the solution b into a hydrothermal reaction kettle to react for 10-16 h at 140-180 ℃ to obtain a product;
d. after the product is cooled, nano-flake Cd is obtained by separation, washing and drying2V2O7And (3) nano materials.
2. The method of claim 1, wherein: in the step d, the separation is centrifugal separation, the washing comprises deionized water washing and absolute ethyl alcohol washing, and the drying is vacuum drying at 90-100 ℃.
3. Cd prepared by the preparation method of claim 1 or 22V2O7And (3) nano materials.
4. Use of Cd as claimed in claim 32V2O7Cd prepared from nano material2V2O7And (3) a composite electrode.
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