CN114715954A - Preparation method and application of NiMn-LDH material after three-dimensional flower-ball-shaped partial vulcanization - Google Patents
Preparation method and application of NiMn-LDH material after three-dimensional flower-ball-shaped partial vulcanization Download PDFInfo
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Abstract
The invention provides a preparation method of a NiMn-LDH material after three-dimensional flower ball-shaped partial vulcanization, which comprises the following steps: dissolving terephthalic acid in N, N-dimethylformamide a, and adding Ni (NO)3)2·6H2O and MnCl2·4H2Adding NaOH aqueous solution into the mixture for hydrothermal reaction, centrifuging the mixture, washing precipitate, and drying the precipitate in vacuum to obtain the aqueous sodium hydroxide solution in which the three-dimensional flower-shaped microspherical NiMn-MOFs material is dissolvedAnd washing the obtained precipitate, then drying in vacuum, dissolving the obtained 3D layered NiMn-LDH material in absolute ethyl alcohol, adding thioacetamide for hydrothermal reaction, washing, and then drying in vacuum to obtain the three-dimensional flower-ball-shaped partially vulcanized NiMn-LDH material. Also provided is an application, which is applied to the positive electrode of the super capacitor. The NiMn-LDH material prepared by the method has high specific capacitance, good rate capability and good cycle stability, and can be widely applied to the positive electrode of a super capacitor.
Description
Technical Field
The invention belongs to the technical field of electrode materials of super capacitors, and particularly relates to a preparation method and application of a NiMn-LDH material after three-dimensional flower-ball-shaped partial vulcanization.
Background
The modern science and technology society requires large-scale use of energy storage devices with large specific capacitance, large power density and clean energy, so that the research of super capacitors becomes a hotspot and also becomes the most important way for relieving or even solving the current situation of the current energy crisis. Super Capacitors (SCs) are unconventional energy devices based on the principle of electrochemical energy conversion, and are novel energy storage devices between rechargeable batteries and conventional capacitors. Compared with the traditional capacitor and lithium ion battery, the Super Capacitor (SCs) has the advantages of low environmental pollution, high power density, good cycle stability, long service life and the like. Therefore, the super capacitor has been widely used in the fields of mobile electronic devices, energy management, hybrid cars, public transportation and memory backup systems, etc., however, the relatively low energy density of the super capacitor severely limits the progress of the commercial application thereof.
Transition metal hydroxide is considered to be a pseudocapacitance material with great application prospect due to the advantages of unique two-dimensional layered structure, high specific capacitance and the like. Layered hydroxide materials are a class of multi-metal hydroxide materials consisting of a positive host layer and intercalated anions/water. Due to the controllable cation composition and the high exchange capacity of anions, the transition metal LDH material always shows excellent electrochemical performance and is widely applied to the super capacitor. The Mn element can be doped to increase the mobility of carriers, so that the binary NiMn-LDH has more excellent electrochemical performance than a single metal hydroxide. However, as an electrode material of a supercapacitor, NiMn-LDH has low specific capacitance and unsatisfactory stability, so that the practical application of NiMn-LDH in the supercapacitor is limited.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method and application of a three-dimensional flower-ball-shaped partially vulcanized NiMn-LDH material aiming at the defects of the prior art.
In order to solve the technical problems, the invention adopts the technical scheme that: a preparation method of a NiMn-LDH material after three-dimensional flower-ball-shaped partial vulcanization comprises the following steps:
s1, dissolving terephthalic acid in N, N-dimethylformamide a, stirring and mixing for 5-15 min, and adding Ni (NO)3)2·6H2O and MnCl2·4H2O, magnetically stirring and mixing for 1-2 h, adding a NaOH aqueous solution with the concentration of 0.4mol/L, performing hydrothermal reaction for 8h at the temperature of 100 ℃, centrifuging, washing the separated precipitate with N, N-dimethylformamide b for 3-5 times, washing with absolute ethyl alcohol for 3-5 times, and after the absolute ethyl alcohol is volatilized, performing vacuum drying for 15h at the temperature of 60 ℃ to obtain the three-dimensional flower-shaped microspherical NiMn-MOFs material;
s2, dissolving the three-dimensional flower-like microspherical NiMn-MOFs material obtained in S1 in a sodium hydroxide aqueous solution with the concentration of 0.5mol/L, mixing the materials for 2 hours through magnetic stirring, washing the obtained precipitate for 3 to 5 times by using ultrapure water, washing the precipitate for 3 to 5 times by using absolute ethyl alcohol, and after the absolute ethyl alcohol is volatilized, carrying out vacuum drying for 15 hours at the temperature of 60 ℃ to obtain a 3D layered NiMn-LDH material;
s3, dissolving the 3D layered NiMn-LDH material obtained in S2 in absolute ethyl alcohol, magnetically stirring for 15-20 min, adding thioacetamide, continuously magnetically stirring for dissolving for 1-2 h, carrying out hydrothermal reaction at 160 ℃ for 6h, centrifuging, washing the precipitate with ultrapure water for 3-5 times, washing with absolute ethyl alcohol for 3-5 times, and after the absolute ethyl alcohol is volatilized, carrying out vacuum drying at 60 ℃ for 15h to obtain the three-dimensional flower-ball-shaped partially vulcanized NiMn-LDH material.
Preferably, terephthalic acid, N-dimethylformamide a, Ni (NO) as described in S13)2·6H2O、MnCl2·4H2The dosage ratio of O to the NaOH aqueous solution with the concentration of 0.4mol/L is 2 mmol: 40mL of: 0.66 mmol: 0.33 mmol: 4 mL.
Preferably, the rotation speed of the centrifugation in the S1 is 2500 r/min-5000 r/min, and the centrifugation time is 5 min-15 min.
Preferably, the dosage ratio of the three-dimensional flower-like microspherical NiMn-MOFs material in S2 to the 0.5mol/L sodium hydroxide aqueous solution is 0.1 g: 2.5 mL.
Preferably, the ratio of the 3D layered NiMn-LDH material and thioacetamide in S3 is 0.02 g: 8 mmol.
Preferably, the rotation speed of the centrifugation in the S3 is 8000r/min, and the centrifugation time is 5 min.
The invention also provides an application of the prepared NiMn-LDH material after the three-dimensional flower-ball-shaped part is vulcanized, and the NiMn-LDH material after the three-dimensional flower-ball-shaped part is vulcanized is applied to a super capacitor anode.
Compared with the prior art, the invention has the following advantages:
the invention provides a method for synthesizing a partially vulcanized NiMn-LDH material in a three-dimensional flower ball shape, which comprises the steps of taking nickel nitrate hexahydrate, manganese chloride tetrahydrate and terephthalic acid as raw materials, synthesizing a NiMn-MOFs material by a hydrothermal method, etching the NiMn-MOFs material by using NaOH aqueous solution to generate the NiMn-LDH material, adding thioacetamide on the basis, and obtaining the partially vulcanized NiMn-LDH material by the hydrothermal method. After the vulcanization process, the edges of the petals are rougher, the size of the petals is smaller, the overall conductivity and the cycling stability of the material are improved, the application value of the electrochemical performance of the supercapacitor is high, the preparation method is simple and convenient, the reaction condition is mild, the requirement on equipment is low, the cost is reduced, NiMn-LDH materials with different vulcanization degrees are prepared, the prepared partially vulcanized NiMn-LDH material has the electrochemical performance of high specific capacitance and good rate capability and cycling stability, and the material is widely applied to the positive electrode of the supercapacitor.
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is an SEM image of a three-dimensional flower-like microspherical NiMn-MOFs material prepared in example 1 of the present invention.
FIG. 2 is an SEM picture of 3D layered NiMn-LDH material prepared in example 1 of the present invention.
FIG. 3 is an XRD pattern of a three-dimensional flower-ball-shaped partially vulcanized NiMn-LDH material prepared in example 1 of the invention and a corresponding standard card.
FIG. 4 is an SEM picture of NiMn-LDH material after the three-dimensional flower ball-shaped part prepared in the invention example 1 is vulcanized.
FIG. 5 is a cyclic voltammogram of the three-dimensional flower-ball-shaped partially vulcanized NiMn-LDH material prepared in example 1 of the invention at different sweeping speeds.
FIG. 6 is a constant current charge and discharge diagram of NiMn-LDH materials after the three-dimensional flower-ball-shaped part is vulcanized, which are prepared in example 1 of the invention, under different current densities.
FIG. 7 is a graph of the cycling performance of the three-dimensional flower-ball-shaped partially vulcanized NiMn-LDH material prepared in example 1 of the present invention.
Detailed Description
Example 1
The preparation method of the three-dimensional flower-ball-shaped partially vulcanized NiMn-LDH material of the embodiment comprises the following steps:
s1, dissolving 2mmol of terephthalic acid in 40mL of N, N-dimethylformamide a, stirring and mixing for 5min, and then adding 0.66mmol of Ni (NO)3)2·6H2O and 0.33mmol of MnCl2·4H2O, magnetically stirring and mixing for 1h, adding 4mL of 0.4mol/L NaOH aqueous solution, performing hydrothermal reaction for 8h at the temperature of 100 ℃, and rotating at the speed of 2500r/minCentrifuging for 5min, washing the separated precipitate with N, N-dimethylformamide b for 3 times, then washing with absolute ethyl alcohol for 3 times, and after the absolute ethyl alcohol is volatilized, vacuum-drying at 60 ℃ for 15h to obtain the three-dimensional flower-like microspherical NiMn-MOFs material;
s2, dissolving 0.1g of the three-dimensional flower-like microspherical NiMn-MOFs material obtained in S1 in 2.5mL of sodium hydroxide aqueous solution with the concentration of 0.5mol/L, mixing the solution by magnetic stirring for 2 hours, washing the obtained precipitate with ultrapure water for 3 times, washing the precipitate with absolute ethyl alcohol for 3 times, and after the absolute ethyl alcohol is volatilized, drying the precipitate in vacuum at the temperature of 60 ℃ for 15 hours to obtain a 3D layered NiMn-LDH material;
s3, dissolving 0.02g of the 3D layered NiMn-LDH material obtained in S2 in absolute ethyl alcohol, magnetically stirring and dissolving for 15min, adding 8mmol of thioacetamide, continuously magnetically stirring and dissolving for 1h, performing hydrothermal reaction at 160 ℃ for 6h, centrifuging at 8000r/min for 5min, washing the precipitate with ultrapure water for 3 times, washing with absolute ethyl alcohol for 3 times, volatilizing the absolute ethyl alcohol, and performing vacuum drying at 60 ℃ for 15h to obtain the three-dimensional flower-ball-shaped partially vulcanized NiMn-LDH material.
The embodiment also provides application of the prepared three-dimensional flower-ball-shaped partially vulcanized NiMn-LDH material, and the three-dimensional flower-ball-shaped partially vulcanized NiMn-LDH material is applied to a supercapacitor positive electrode.
FIG. 1 is an SEM image of the three-dimensional flower-like microspherical NiMn-MOFs material prepared in this example, and as shown in FIG. 1, the NiMn-MOFs material has a regular flower-ball shape and is fully covered with fine lamellae on the surface. Has a large specific surface area.
Fig. 2 is an SEM image of the 3D layered NiMn-LDH material prepared in this example, which, as shown in fig. 2, is composed of many interlaced petal-shaped nanosheets, substantially retaining the overall morphology of the MOFs precursors. And it is also evident that the edges of the sheet start to have a curvature, similar to a petal. The initially straight and upstanding nanosheets in NiMn-MOFs exhibit wavy bends, which may be attributed to the large surface energy of the LDH sheets.
Fig. 3 is an XRD pattern of the three-dimensional flower-ball-shaped partially-vulcanized NiMn-LDH material prepared in this example, and as shown in the figure, the diffraction peaks of the partially-vulcanized NiMn-LDH at 2 θ of 30.96 °, 34.75 °, 38.47 °, 44.60 ° and 53.08 ° can be attributed to (200), (210), (211), (220) and (311) plane cubic phases NiS2(JCPDS No. 89-1495). The diffraction peak of the NiMn-LDH material after partial vulcanization at the 2 theta of 19.91 DEG can be attributed to the characteristic diffraction peak of the (006) crystal face, which is the characteristic diffraction peak of the LDH, and the prepared material is the NiMn-LDH material after partial vulcanization.
Fig. 4 is an SEM image of the partially vulcanized NiMn-LDH material in three-dimensional flower ball shape prepared in this example, as shown in fig. 4, on the basis of maintaining the three-dimensional flower-like microspherical shape of the NiMn-MOFs material, LDH has a micro-leaf-like morphology, mainly consisting of nano-sheet "petals", and the edges of the petals are rougher after the vulcanization process, and the size of the "petals" is smaller.
FIG. 5 is a cyclic voltammogram of the three-dimensional flower-ball-shaped partially-vulcanized NiMn-LDH material prepared in the embodiment at different sweep rates, as shown in FIG. 3, a significant redox peak can be seen through a CV curve, and thus the material can be proved to be a typical pseudocapacitive material;
in addition, as the sweep rate is increased, the peak current of the redox peak is obviously increased, which indicates that the redox rate on the electrode is increased;
meanwhile, the integral shape of the curve is not changed greatly, and the corresponding redox peak is kept better, which indicates that the polarization phenomenon of the electrode is not obvious.
FIG. 6 is the constant current charge-discharge diagram of the NiMn-LDH material after the three-dimensional flower ball shape partial vulcanization prepared in the example under different current densities, as shown in FIG. 6, at 0.5, 1, 2, 5, 10, 20 A.g-1The specific capacitances at different current densities are 1387, 1202, 1136, 820, 580, 260F g-1The material has higher specific capacitance.
FIG. 7 is a graph of the cycle performance of the partially vulcanized NiMn-LDH material in the three-dimensional flower ball shape prepared in the example, and as shown in FIG. 7, the specific capacitance of the partially vulcanized NiMn-LDH material can still maintain the initial 74.3% after 1000 cycles, which shows that the material has better cycle stability.
Example 2
The preparation method of the NiMn-LDH material vulcanized by the three-dimensional flower-ball-shaped part of this embodiment comprises the following steps:
s1, dissolving 2mmol of terephthalic acid in 40mL of N, N-dimethylformamide a, stirring and mixing for 15min, and adding 0.66mmol of Ni (NO)3)2·6H2O and 0.33mmol of MnCl2·4H2O, magnetically stirring and mixing for 2 hours, adding 4mL of NaOH aqueous solution with the concentration of 0.4mol/L, performing hydrothermal reaction for 8 hours at the temperature of 100 ℃, centrifuging for 5 minutes at the rotating speed of 5000r/min, washing the separated precipitate for 5 times by using N, N-dimethylformamide b, washing for 5 times by using absolute ethyl alcohol, and after the absolute ethyl alcohol is volatilized, performing vacuum drying for 15 hours at the temperature of 60 ℃ to obtain the three-dimensional flower-shaped microspherical NiMn-MOFs material;
s2, dissolving 0.1g of the three-dimensional flower-like microspherical NiMn-MOFs material obtained in S1 in 2.5mL of sodium hydroxide aqueous solution with the concentration of 0.5mol/L, mixing the solution by magnetic stirring for 2 hours, washing the obtained precipitate for 5 times by using ultrapure water, washing the precipitate for 5 times by using absolute ethyl alcohol, and drying the precipitate for 15 hours in vacuum at the temperature of 60 ℃ after the absolute ethyl alcohol is volatilized to obtain a 3D layered NiMn-LDH material;
s3, dissolving 0.02g of the 3D layered NiMn-LDH material obtained in S2 in absolute ethyl alcohol, magnetically stirring and dissolving for 20min, adding 8mmol of thioacetamide, continuously magnetically stirring and dissolving for 2h, carrying out hydrothermal reaction for 6h at 160 ℃, centrifuging for 5min at 8000r/min, washing the precipitate with ultrapure water for 5 times, washing with absolute ethyl alcohol for 5 times, volatilizing the absolute ethyl alcohol, and carrying out vacuum drying for 15h at 60 ℃ to obtain the three-dimensional flower-ball-shaped partially vulcanized NiMn-LDH material.
The NiMn-LDH material prepared by the three-dimensional flower-ball-shaped part vulcanization in the embodiment is applied to a super capacitor anode. On the basis of the electrode material of the NiMn-LDH material after partial sulfuration, taking AC as negativeAnd the partially vulcanized NiMn-LDH is used as the positive electrode, the partially vulcanized NiMn-LDH// AC HSC is constructed, and the electrochemical performance of the partially vulcanized NiMn-LDH// AC HSC is researched. The partially vulcanized NiMn-LDH// AC HSC is subjected to GCD test, and when the current density is 1 A.g-1、2A·g-1、3A·g-1、5A·g-1And 10A. g-1The specific capacitance is 121.2F g-1、96.5F·g-1、81.9F·g-1、64.8F·g-1And 47.1 Fg-1。
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (7)
1. A preparation method of a NiMn-LDH material after three-dimensional flower-ball-shaped partial vulcanization is characterized by comprising the following steps:
s1, dissolving terephthalic acid in N, N-dimethylformamide a, stirring and mixing for 5-15 min, and adding Ni (NO)3)2·6H2O and MnCl2·4H2O, magnetically stirring and mixing for 1-2 h, adding a NaOH aqueous solution with the concentration of 0.4mol/L, performing hydrothermal reaction for 8h at the temperature of 100 ℃, centrifuging, washing the separated precipitate with N, N-dimethylformamide b for 3-5 times, washing with absolute ethyl alcohol for 3-5 times, and after the absolute ethyl alcohol is volatilized, performing vacuum drying for 15h at the temperature of 60 ℃ to obtain the three-dimensional flower-shaped microspherical NiMn-MOFs material;
s2, dissolving the three-dimensional flower-like microspherical NiMn-MOFs material obtained in S1 in a sodium hydroxide aqueous solution with the concentration of 0.5mol/L, mixing the materials for 2 hours through magnetic stirring, washing the obtained precipitate for 3 to 5 times by using ultrapure water, washing the precipitate for 3 to 5 times by using absolute ethyl alcohol, and after the absolute ethyl alcohol is volatilized, carrying out vacuum drying for 15 hours at the temperature of 60 ℃ to obtain a 3D layered NiMn-LDH material;
s3, dissolving the 3D layered NiMn-LDH material obtained in S2 in absolute ethyl alcohol, magnetically stirring for 15-20 min, adding thioacetamide, continuously magnetically stirring for dissolving for 1-2 h, carrying out hydrothermal reaction at 160 ℃ for 6h, centrifuging, washing the precipitate with ultrapure water for 3-5 times, washing with absolute ethyl alcohol for 3-5 times, and after the absolute ethyl alcohol is volatilized, carrying out vacuum drying at 60 ℃ for 15h to obtain the three-dimensional flower-ball-shaped partially vulcanized NiMn-LDH material.
2. The method for preparing the NiMn-LDH material after the three-dimensional flower-ball-shaped partial vulcanization according to claim 1, wherein the terephthalic acid, N-dimethylformamide a and Ni (NO) are contained in S13)2·6H2O、MnCl2·4H2The dosage ratio of O to the NaOH aqueous solution with the concentration of 0.4mol/L is 2 mmol: 40mL of: 0.66 mmol: 0.33 mmol: 4 mL.
3. The method for preparing the NiMn-LDH material after the three-dimensional flower-ball-shaped partial vulcanization according to claim 1, wherein the rotation speed of centrifugation in S1 is 2500 r/min-5000 r/min, and the time of centrifugation is 5 min-15 min.
4. The method for preparing the NiMn-LDH material after the three-dimensional flower-shaped spherical part is vulcanized according to claim 1, wherein the dosage ratio of the three-dimensional flower-shaped microspherical NiMn-MOFs material in S2 to the 0.5mol/L sodium hydroxide aqueous solution is 0.1 g: 2.5 mL.
5. The method for preparing the NiMn-LDH material after the three-dimensional flower-ball-shaped partial vulcanization according to claim 1, wherein the dosage ratio of the 3D layered NiMn-LDH material and thioacetamide in S3 is 0.02 g: 8 mmol.
6. The method for preparing the NiMn-LDH material after the three-dimensional flower-ball-shaped partial vulcanization according to claim 1, wherein the rotation speed of centrifugation in S3 is 8000r/min, and the time of centrifugation is 5 min.
7. Use of a three-dimensional flower-ball-shaped partially sulphided NiMn-LDH material prepared according to any of claims 1-6, in a supercapacitor positive electrode.
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