CN114530599A - Polyaniline modified vanadium pentoxide nanosheet material and preparation method and application thereof - Google Patents
Polyaniline modified vanadium pentoxide nanosheet material and preparation method and application thereof Download PDFInfo
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 71
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical class [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000000463 material Substances 0.000 title claims abstract description 66
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 78
- 239000011259 mixed solution Substances 0.000 claims abstract description 34
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 32
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000011229 interlayer Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- 239000011149 active material Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 230000002441 reversible effect Effects 0.000 abstract description 2
- 239000006183 anode active material Substances 0.000 abstract 1
- 239000007774 positive electrode material Substances 0.000 description 12
- 150000002500 ions Chemical class 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 8
- 239000010410 layer Substances 0.000 description 6
- 239000002033 PVDF binder Substances 0.000 description 5
- 238000000840 electrochemical analysis Methods 0.000 description 5
- 239000007772 electrode material Substances 0.000 description 5
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000002064 nanoplatelet Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical group [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- 239000006245 Carbon black Super-P Substances 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009831 deintercalation Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 229910052760 oxygen Chemical group 0.000 description 1
- 239000001301 oxygen Chemical group 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The invention provides a polyaniline modified vanadium pentoxide nanosheet material, and a preparation method and application thereof, wherein the preparation method comprises the following steps: adding vanadium pentoxide powder into deionized water, uniformly mixing, and adding aniline to form a mixed solution A; dripping hydrochloric acid into the mixed solution A, adjusting the pH value to acidity, and stirring to obtain a mixed solution B; and (3) placing the mixed solution B into a high-pressure reaction kettle for hydrothermal reaction, and then cooling, washing and drying to obtain the polyaniline modified vanadium pentoxide nanosheet material. The polyaniline modified vanadium pentoxide nanosheet material provided by the invention is stable in structure, shows good electrochemical performance when used as an ammonium ion battery anode active material, and has high reversible charge-discharge specific capacity.
Description
Technical Field
The invention relates to the technical field of detection and analysis of environmental pollutants, in particular to a polyaniline modified vanadium pentoxide nanosheet material and a preparation method and application thereof.
Background
The non-metal carrier is a choice for replacing metal ions in the water-based battery, and has the advantages of fast kinetics, long cycle life, low manufacturing cost and the like. NH (NH)4 +The ions have some unique properties as charge carriers, exhibiting the lightest molar mass, only 18gmol-1. Although it has
(CN. about.6) large ionic radius, but NH4 +The hydrated ion size of the ions is minimal, facilitating rapid diffusion thereof in the aqueous electrolyte. In addition, with H+Acid electrolyte ratio of the battery, NH4 +The electrolyte exhibits weak acidity and less corrosiveness, does not cause dissolution of electrode materials, and contains H+Has a higher HER overpotential. Due to NH4 +Radius ratio of ion H+Large ions, the electrode material needs more space to accommodate NH during intercalation/deintercalation4 +Ions, which can cause a significant change in the electrode structure. Therefore, the performance requirements of ammonium ion batteries on the electrode material are high, which greatly limits NH4 +The development of batteries.
Vanadium pentoxide has the advantages of high capacity, abundant reserves, low cost and the like, and is considered to be a very competitive next-generation electrode material. Orthorhombic vanadium pentoxide (space group: Pmmn; unit cell parameters:
) Is a typical layered structure, is VO formed by 5V-O bonds formed by vanadium atoms and oxygen atoms5The square pyramid is formed by connecting a common edge and a common point on an ab crystal face. Because of the larger distance between vanadium pentoxide layers, the method is suitable for Li+、Na+、Mg2+The plasma is embedded and removed, so that the energy storage material is applied.
However, there is no report on the use of vanadium pentoxide as an electrode material for ammonium ion batteries.
Disclosure of Invention
In view of the above, the invention provides a polyaniline modified vanadium pentoxide nanosheet material, and a preparation method and an application thereof, so as to solve the problem that the existing ammonium ion battery anode material is low in specific capacity.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a preparation method of a polyaniline modified vanadium pentoxide nanosheet material comprises the following steps:
s1, adding vanadium pentoxide powder into deionized water, uniformly mixing, and adding aniline to form a mixed solution A;
s2, dripping hydrochloric acid into the mixed solution A, adjusting the pH value to acidity, and stirring to obtain mixed solution B;
and S3, placing the mixed solution B in a high-pressure reaction kettle for hydrothermal reaction, and then cooling, washing and drying to obtain the polyaniline modified vanadium pentoxide nanosheet material.
Further, in the mixed solution a in step S1, the mass ratio of the vanadium pentoxide to the aniline is in the range of 1:1 to 1: 3.
Further, in step S2, the pH of mixed solution B is in the range of 2 to 4.
Further, in step S2, the concentration of hydrochloric acid is in the range of 2M to 4M.
Further, in step S2, the stirring time is in the range of 25min to 35 min.
Further, in step S3, the temperature of the hydrothermal reaction is in the range of 120 ℃ to 110 ℃ and the reaction time is in the range of 12h to 24 h.
The second purpose of the invention is to provide a polyaniline-modified vanadium pentoxide nanosheet material, which is prepared by the preparation method of the polyaniline-modified vanadium pentoxide nanosheet material.
Further, the polyaniline modified vanadium pentoxide nanosheet material is of a layered structure.
Further, the interlayer spacing of the polyaniline modified vanadium pentoxide nanosheet material is in the range of 1nm to 2 nm.
The third objective of the present invention is to provide an application of the polyaniline-modified vanadium pentoxide nanosheet material as an active material of an anode of an ammonium ion battery.
Compared with the prior art, the invention has the following advantages:
(1) the polyaniline modified vanadium pentoxide nanosheet material provided by the invention is stable in structure, shows good electrochemical performance when used as an ammonium ion battery positive electrode active material, and has an electrochemical performance of 500mAg-1The current density of the lithium ion battery is higher in reversible charge-discharge specific capacity.
(2) The preparation method is simple, the raw materials are cheap and easy to obtain, and the preparation method is suitable for large-scale production.
Drawings
In order to more clearly illustrate the technical solutions of the present invention or the prior art, some brief descriptions will be given below to the drawings used in the description of the embodiments or the prior art, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is an XRD (X-ray diffraction) pattern of a polyaniline-modified vanadium pentoxide nanosheet material according to example 1 of the present invention;
FIG. 2 is an SEM image of a polyaniline-modified vanadium pentoxide nanosheet material in example 1 of the present invention;
FIG. 3 is a TEM image of the polyaniline-modified vanadium pentoxide nanosheet material of embodiment 1 of the present invention;
FIG. 4 is an HRTEM image of a polyaniline-modified vanadium pentoxide nanosheet material according to example 1 of the present invention;
FIG. 5 is an FTIR chart of the polyaniline-modified vanadium pentoxide nanoplatelets according to example 1 of the present invention;
fig. 6 is a constant current charge-discharge performance diagram of an ammonium ion battery assembled by a polyaniline-modified vanadium pentoxide nanosheet material in embodiment 1 of the present invention;
fig. 7 is a rate performance diagram of an ammonium ion battery assembled by the polyaniline-modified vanadium pentoxide nanosheet material in embodiment 1 of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
It should be noted that in the description of the embodiments herein, the description of the term "some embodiments" means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. Throughout this specification, the schematic representations of the terms used above do not necessarily refer to the same implementation or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. The term "in.. range" includes both ends, such as "in the range of 1 to 100" includes both 1 and 100 ends.
The embodiment of the invention provides a preparation method of a polyaniline modified vanadium pentoxide nanosheet material, which comprises the following steps:
s1, adding vanadium pentoxide powder into deionized water, uniformly mixing, and adding aniline to form a mixed solution A;
s2, dripping hydrochloric acid into the mixed solution A, adjusting the pH value to acidity, and stirring to obtain a mixed solution B;
and S3, placing the mixed solution B in a high-pressure reaction kettle for hydrothermal reaction, cooling, washing and drying to obtain the polyaniline modified vanadium pentoxide nanosheet material.
It can be understood that the vanadium pentoxide layers are connected by weak van der waals interaction, so that ions or molecules can be inserted to form derivative compounds, and the interlayer spacing can be enlarged by embedding the ions or small molecules, so that a wider ion transmission channel can be obtained.
Therefore, the polyaniline modified vanadium pentoxide nanosheet is prepared by a hydrothermal method, polyaniline micromolecules are embedded between vanadium pentoxide layers, the distance between the vanadium pentoxide layers is enlarged, and a wide interlayer space can expose more storage sites and provide more ammonium storage capacity, so that the polyaniline modified vanadium pentoxide nanosheet can show good electrochemical performance when used as an active material of an anode of an ammonium ion battery.
Specifically, in step S1, the mass ratio of vanadium pentoxide to aniline in the mixed solution a is in the range of 1:1 to 1: 3.
In step S2, hydrochloric acid is dropped into the mixed solution A, the pH value of the solution system is adjusted within the range of 2-4, and the mixed solution B is obtained after stirring for 25min to 35 min.
Wherein the concentration of hydrochloric acid is in the range of 2M to 4M, preferably the concentration of hydrochloric acid is 3M.
Specifically, in step S3, the hydrothermal reaction temperature is in the range of 120 ℃ to 110 ℃ and the reaction time is in the range of 12h to 24 h.
Therefore, the preparation method is simple, the raw materials are cheap and easy to obtain, and the preparation method is suitable for large-scale production.
The invention further provides a polyaniline-modified vanadium pentoxide nanosheet material, which is prepared by the preparation method of the polyaniline-modified vanadium pentoxide nanosheet material.
Wherein, the polyaniline modified vanadium pentoxide nanosheet material is of a layered structure, and the interlayer spacing thereof is within the range of 1nm to 2 nm.
The invention further provides an application of the polyaniline-modified vanadium pentoxide nanosheet material as an active material of an ammonium ion battery anode.
The interlayer spacing of vanadium pentoxide is increased by embedding polyaniline between vanadium pentoxide layers, so that when the polyaniline modified vanadium pentoxide nanosheet material is used as an ammonium ion battery positive electrode material, the polyaniline modified vanadium pentoxide nanosheet material can show higher specific capacity and excellent rate capability.
On the basis of the above embodiment, the present invention provides the following specific example of the preparation method of the polyaniline-modified vanadium pentoxide nanosheet material, and further illustrates the present invention. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are examples of experimental procedures not specified under specific conditions, generally according to the conditions recommended by the manufacturer. Unless otherwise indicated, percentages and parts are by mass.
Example 1
The embodiment provides a preparation method of a polyaniline-modified vanadium pentoxide nanosheet material, which comprises the following steps:
1) adding 0.1814g of vanadium pentoxide powder into 30mL of deionized water at room temperature, continuously stirring, and then dripping 60 mu L of aniline to obtain a mixed solution A;
2) dropwise adding 3M HCl into the mixed solution A, adjusting the pH value to 3, and continuously stirring for 30min to obtain a mixed solution B;
3) and transferring the mixed solution B into a 50mL Teflon-lined stainless steel autoclave, reacting in an oven at 120 ℃ for 24h, cooling in the air after the reaction is finished, washing with deionized water and ethanol after cooling, and drying to obtain the polyaniline modified vanadium pentoxide nanosheet material.
And (3) carrying out morphology analysis and element analysis on the polyaniline modified vanadium pentoxide nanosheet material to obtain a result graph as shown in figures 1-5.
FIG. 1 is an X-ray diffraction (XRD) pattern of the polyaniline-modified vanadium pentoxide nanoplatelets, from which it can be seen that (00l) series of peaks exist on the pattern, indicating the layered structure of the polyaniline-modified vanadium pentoxide nanoplatelets, and it can be deduced that the interlayer spacing thereof is about 1.55 nm.
Fig. 2 is a Field Emission Scanning Electron Microscope (FESEM) image of the polyaniline-modified vanadium pentoxide nanosheet material, and it can be seen from the image that the polyaniline-modified vanadium pentoxide nanosheet material is in the form of stacked nanosheets connected at one end.
Fig. 3 is a Transmission Electron Microscope (TEM) image of the polyaniline-modified vanadium pentoxide nanosheet material, from which it can be seen that the polyaniline-modified vanadium pentoxide nanosheet material is in the form of an extremely thin nanosheet.
FIG. 4 is a high-resolution transmission electron microscope (HRTEM) of a polyaniline-modified vanadium pentoxide nanosheet material, and as can be seen from the graph, the lattice spacing of the polyaniline-embedded nanosheets is 1.55 nm.
FIG. 5 is a Fourier Transform Infrared (FTIR) test chart of the polyaniline-modified vanadium pentoxide nanosheet material, and it can be seen from the chart that the presence of polyaniline is proved by characteristic peaks obtained in the wavelength range of 1000-1500, which proves the successful intercalation of polyaniline.
In conclusion of the morphological analysis and the elemental analysis, it can be seen that after polyaniline is embedded, vanadium pentoxide shows a very large interlayer spacing, so that NH can be supplied4 +The insertion and extraction provides more spatial sites.
The polyaniline-modified vanadium pentoxide nanosheet material prepared in example 1 is used as an ammonium ion battery positive electrode active material, an ammonium ion battery is assembled, and an electrochemical test is performed to obtain a result graph as shown in fig. 6 and fig. 1.
The specific assembling method of the ammonium ion battery comprises the following steps: using polyaniline modified vanadium pentoxide nanosheet material as a working electrode, using a platinum sheet electrode as a counter electrode, using a Saturated Calomel Electrode (SCE) as a reference electrode, and selecting 0.5M (NH)4)2SO4The solution serves as an electrolyte.
As can be seen from FIG. 6, the first discharge specific capacity of the ammonium ion battery is 301mAh g-1The first charging specific capacity is 215mAh g-1The first coulombic efficiency was found to be 89.5%.
As can be seen from figure 1, the polyaniline modified vanadium pentoxide nanosheet material shows a relatively fast ammonium ion transmission performance, and the ammonium ion battery has a good rate capability of 10A g-1At a current density of 100mAh g-1The specific capacity of (a).
The test result shows that the polyaniline modified vanadium pentoxide nanosheet material has excellent electrochemical performance and is a potential high-performance ammonium ion battery positive electrode material.
Example 2
The embodiment provides a preparation method of a polyaniline-modified vanadium pentoxide nanosheet material, which comprises the following steps:
1) adding 0.1814g of vanadium pentoxide powder into 30mL of deionized water at room temperature, continuously stirring, and then dripping 30 mu L of aniline to obtain a mixed solution A;
2) dropwise adding 3M HCl into the mixed solution A, adjusting the pH value to 3, and continuously stirring for 30min to obtain a mixed solution B;
3) transferring the mixed solution B into a 50mL Teflon-lined stainless steel autoclave, reacting in an oven at 120 ℃ for 24h, cooling in the air after the reaction is finished, washing with deionized water and ethanol after cooling, and drying to obtain a polyaniline modified vanadium pentoxide nanosheet material;
4) mixing polyaniline modified vanadium pentoxide nanosheets, ultra-dense high-conductivity carbon black Super P and polyvinylidene fluoride PVDF according to the ratio of 1:2:1, pulping, and coating the mixture on carbon paper to obtain the ammonium-based positive electrode material of the sub-battery.
An ammonium ion battery was assembled from the positive electrode material of the ammonium ion battery prepared in example 2, and an electrochemical test was performed. The results show that at 500mAg-1Under the current density, the first discharge specific capacity can reach 152mAh g-1At 10A g-1Under the current density, the first discharge specific capacity can reach 40mAh g-1。
Through analysis, the interlayer spacing cannot be fully enlarged due to insufficient aniline, the performance of the polyaniline modified vanadium pentoxide nanosheet material is influenced, and further the electrochemical performance is weakened.
Example 3
The embodiment provides a preparation method of a polyaniline-modified vanadium pentoxide nanosheet material, which is different from that in embodiment 1 in that:
in the step 1), 120 mu L of aniline is dripped to obtain a mixed solution A;
the remaining steps and parameters were the same as in example 1.
The polyaniline modified vanadium pentoxide nanosheet material prepared in the embodiment 3, Super P and PVDF are mixed according to the ratio of 1:2:1 to prepare pulp, and the pulp is coated on carbon paper to prepare the positive electrode material of the ammonium ion battery.
To make sureThe positive electrode material of the ammonium ion battery prepared in example 3 was assembled into an ammonium ion battery, and an electrochemical test was performed. The results show that at 500mA g-1The first discharge specific capacity can reach 181mAh g under the current density-1At 10A g-1The first discharge specific capacity can reach 52mAh g under the current density-1。
Through analysis, the reason for the capacity reduction in the example is presumed to be that excessive polyaniline is formed on the surface of the vanadium pentoxide nanosheet due to excessive aniline, and the structural stability is reduced due to excessive interlayer spacing, so that the electrochemical performance of the polyaniline modified vanadium pentoxide nanosheet material is influenced.
Example 4
The embodiment provides a preparation method of a polyaniline-modified vanadium pentoxide nanosheet material, which is different from that in embodiment 1 in that:
in the step 2), dropwise adding 3M HCl into the mixed solution A, and adjusting the pH value to 1;
the remaining steps and parameters were the same as in example 1.
The polyaniline modified vanadium pentoxide nanosheet material prepared in the embodiment 4, Super P and PVDF are mixed according to the ratio of 1:2:1 to prepare pulp, and the pulp is coated on carbon paper to prepare the positive electrode material of the ammonium ion battery.
An ammonium ion battery was assembled from the positive electrode material of the ammonium ion battery prepared in example 4, and an electrochemical test was performed. The results show that at 500mA g-1Under the current density, the first discharge specific capacity can reach 200mAh g-1At 10A g-1Under the current density, the first discharge specific capacity can reach 96mAh g-1。
Through analysis, the fact that when the pH value is too low, polymerization reaction is mainly generated, so that aniline is polymerized before entering a vanadium pentoxide layer, and the electrochemical performance of the polyaniline modified vanadium pentoxide nanosheet material is affected.
Example 5
The embodiment provides a preparation method of a polyaniline-modified vanadium pentoxide nanosheet material, which is different from that in embodiment 1 in that:
in the step 2), dropwise adding 3M HCl into the mixed solution A, and adjusting the pH value to 5;
the remaining steps and parameters were the same as in example 1.
The polyaniline-modified vanadium pentoxide nanosheet material prepared in example 5, Super P and PVDF were mixed in a ratio of 1:2:1, slurried, and coated onto carbon paper to obtain an ammonium-based positive electrode material for a secondary cell.
An ammonium ion battery was assembled from the positive electrode material for an ammonium ion battery prepared in example 5, and an electrochemical test was performed. The results show that at 500mA g-1Under the current density, the first discharge specific capacity can reach 103mAh g-1At 10A g-1Under the current density, the first discharge specific capacity can reach 42mAh g-1。
Through analysis, the vanadium gel can form a flocculation bag structure with extremely tight combination when the pH is 5, and when the pH is too high, the polymerization rate of polyaniline is reduced, so that the electrochemical performance of the polyaniline modified vanadium pentoxide nanosheet material is influenced.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Various changes and modifications may be effected therein by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present disclosure, and these changes and modifications are intended to be within the scope of the present disclosure.
Claims (10)
1. A preparation method of a polyaniline modified vanadium pentoxide nanosheet material is characterized by comprising the following steps:
s1, adding vanadium pentoxide powder into deionized water, uniformly mixing, and adding aniline to form a mixed solution A;
s2, dripping hydrochloric acid into the mixed solution A, adjusting the pH value to acidity, and stirring to obtain mixed solution B;
and S3, placing the mixed solution B in a high-pressure reaction kettle for hydrothermal reaction, and then cooling, washing and drying to obtain the polyaniline modified vanadium pentoxide nanosheet material.
2. The preparation method according to claim 1, wherein in the mixed solution a of step S1, the mass ratio of the vanadium pentoxide to the aniline is in a range from 1:1 to 1: 3.
3. The method according to claim 2, wherein in step S2, the pH of mixed solution B is in the range of 2 to 4.
4. The method according to claim 3, wherein the hydrochloric acid has a concentration in the range of 2M to 4M in step S2.
5. The method according to claim 4, wherein in step S2, the stirring time is in the range of 25min to 35 min.
6. The method according to any one of claims 1 to 5, wherein in step S3, the hydrothermal reaction temperature is in the range of 120 ℃ to 170 ℃ and the reaction time is in the range of 12h to 24 h.
7. A polyaniline-modified vanadium pentoxide nanosheet material, characterized by being prepared by the method for preparing the polyaniline-modified vanadium pentoxide nanosheet material according to any one of claims 1-6.
8. The polyaniline-modified vanadium pentoxide nanosheet material of claim 7, wherein the polyaniline-modified vanadium pentoxide nanosheet material is a layered structure.
9. The polyaniline-modified vanadium pentoxide nanosheet material of claim 7, wherein the interlayer spacing of the polyaniline-modified vanadium pentoxide nanosheet material is in the range of 1nm to 2 nm.
10. Use of the polyaniline-modified vanadium pentoxide nanosheet material of any one of claims 7-9 as an active material for an anode of an ammonium ion battery.
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