CN113307312A - Method for treating cobalt-chromium-nickel hydrotalcite supercapacitor electrode material by alkali-sulfur composite treatment - Google Patents
Method for treating cobalt-chromium-nickel hydrotalcite supercapacitor electrode material by alkali-sulfur composite treatment Download PDFInfo
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Abstract
本发明公开了一种碱硫复合处理钴铬镍水滑石超级电容电极材料的方法，包括以下步骤：首先通过水热法制备钴铬镍水滑石前驱体，然后将钴铬镍水滑石粉末加入NaOH溶液和Na2S溶液按一定比例混合形成均匀的碱硫复合溶液中，在常温常压下搅拌，实现对钴铬镍水滑石的刻蚀与硫化。在碱、硫复合处理过程中，由于刻蚀作用使Cr3+被NaOH溶解形成晶格缺陷，促进离子扩散速率，而硫化作用使钴铬镍水滑石生成无定型硫化物。本发明制备方法简单，成本低廉，制备的超级电容器材料的电化学性能优良，在电势0‑0.7V内，1A/g的电流密度下，与未处理的钴铬镍水滑石相比，碱硫复合处理后最佳比电容从955.1F/g增加到1501.3F/g。在电流密度为20A/g时，倍率性能由48.81％增加到64.63％。
The invention discloses a method for alkali-sulfur composite treatment of cobalt-chromium-nickel hydrotalcite supercapacitor electrode material. The solution and the Na 2 S solution are mixed in a certain proportion to form a uniform alkali-sulfur composite solution, and stirred at normal temperature and pressure to realize the etching and vulcanization of cobalt-chromium-nickel hydrotalcite. In the process of alkali-sulfur compound treatment, Cr 3+ was dissolved by NaOH to form lattice defects due to etching, which promoted the ion diffusion rate, while sulfidation caused cobalt-chromium-nickel hydrotalcite to form amorphous sulfide. The preparation method of the invention is simple, the cost is low, and the prepared supercapacitor material has excellent electrochemical performance. In the potential of 0-0.7V, under the current density of 1A/g, compared with the untreated cobalt-chromium-nickel hydrotalcite, the alkali sulfur The optimum specific capacitance increased from 955.1F/g to 1501.3F/g after compound treatment. When the current density is 20A/g, the rate capability increases from 48.81% to 64.63%.
Description
Technical Field
The invention belongs to the technical field of capacitor electrodes, and particularly relates to a method for treating a cobalt-chromium-nickel hydrotalcite super capacitor electrode material by alkali-sulfur composite treatment.
Background
In the era of increasing demand of renewable energy, the exploration of new storage and conversion technologies becomes an important way to solve the problem of efficient utilization of renewable energy. Among the numerous storage and conversion technologies, electrochemical energy storage is considered to be the most promising of the various renewable energy storage technologies due to its high efficiency and flexibility. Super capacitors have been widely studied due to their extremely strong charge storage capacity and high cycle stability.
The transition metal hydrotalcite material has the advantages of high theoretical specific capacitance, adjustable structural components, environmental protection and the like, so that the transition metal hydrotalcite material becomes a pseudo-capacitance electrode material with great potential. However, the hydrotalcite electrode material has the defects of poor conductivity and easy agglomeration, so that ion transport channels are reduced, and therefore, the optimization of the structure of the hydrotalcite material to improve the electrochemical conductivity of the hydrotalcite material is very important for improving the electrochemical performance of the hydrotalcite material.
Disclosure of Invention
Based on the defects of the prior art, the technical problem to be solved by the invention is to provide the method for alkali-sulfur composite treatment of the cobalt-chromium-nickel hydrotalcite super-capacitor electrode material, the preparation process is simple, the preparation period is short, the price is low, and the capacitance performance of the cobalt-chromium-nickel high hydrotalcite is improved by the simple process method; the material prepared after the alkali and sulfur composite treatment has the advantages of high specific capacity, high rate capability and high stability.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention provides a method for treating a cobalt-chromium-nickel hydrotalcite supercapacitor electrode material by alkali-sulfur composite treatment, which comprises the following steps:
s1, preparing a reaction solution: preparing a mixed solution of 38mmol/L cobalt metal salt solution, 19mmol/L chromium metal salt solution, 13mmol/L nickel metal salt solution and 50mmol/L precipitator, and stirring uniformly by using a magnetic stirrer;
s2, hydrothermal reaction: putting the prepared solution into a reaction kettle, sealing, heating to 160 ℃, and preserving heat for 4 hours;
s3, post-processing: washing a product in the filtering reaction kettle by using water and ethanol to obtain a filter cake, putting the filter cake into a drying oven to be dried at 60 ℃, and then grinding the filter cake to obtain cobalt-chromium-nickel hydrotalcite powder;
s4, preparing an alkali and sulfur composite solution: mixing 1-4mol/L NaOH solution and 2mol/L Na2Mixing the S solution according to the ratio of 2:1, and stirring the mixture uniformly by using a magnetic stirrer;
s5, adding 0.6g of cobalt chromium nickel hydrotalcite powder into the alkali and sulfur composite solution, and stirring for 24 hours at normal temperature and normal pressure to obtain the cobalt chromium nickel hydrotalcite powder subjected to alkali and sulfur composite treatment.
In the invention, hydrotalcite is synthesized first, and then hydrotalcite is chemically treated to produce crystal defects, which is an effective means for improving the capacitive performance of hydrotalcite. Cr (OH)3Is an amphoteric substance, and can be dissolved in a strong alkaline solution. Cr (OH)3With OH-The reaction generates soluble material Cr (OH)4 -The chemical reaction equation of (a) is:
Cr(OH)3+OH-＝Cr(OH)4 -
the invention can solve the defects of poor conductivity and low rate capability of the existing Cr-containing hydrotalcite in the application aspect of the super capacitor. The invention firstly synthesizes the cobalt-chromium-nickel hydrotalcite, and then utilizes strong alkali to treat the cobalt-chromium-nickel hydrotalcite to dissolve part of Cr so as to cause defects of the hydrotalcite material, improve the ion diffusion rate and improve the electrochemical performance.
The cobalt-chromium-nickel hydrotalcite is vulcanized to generate amorphous sulfide, and the sulfide containing Ni and Co has the advantages of higher intrinsic conductivity, larger specific surface area and higher theoretical capacity compared with hydroxide, and can obtain higher capacitance performance.
According to the invention, the cobalt-chromium-nickel hydrotalcite is used as a precursor, and the composite material of the amorphous sulfide with lattice defects and the cobalt-chromium-nickel hydrotalcite is prepared by an alkali-sulfur composite treatment method. The generation of lattice defects promotes the ion diffusion rate during the redox reaction, and the generation of sulfides improves the conductivity of the material, so that the capacitance performance of the hydrotalcite material treated by alkali and sulfur in a compounding way is improved. Through electrochemical tests, compared with untreated cobalt chromium nickel hydrotalcite, the specific capacitance of the treated cobalt chromium nickel hydrotalcite material is increased by 1.7 times, and the rate capability is also improved. Meanwhile, in the aspect of the process, the process method for the alkali and sulfur composite treatment is simple to operate, and the effect better meets the expected standard.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the content of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following detailed description is given in conjunction with the preferred embodiments, together with the accompanying drawings.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings of the embodiments will be briefly described below.
FIG. 1 is an XRD pattern of cobalt-chromium-nickel hydrotalcite prepared in example 1 before and after an alkali-sulfur composite treatment;
FIG. 2 is SEM images of cobalt-chromium-nickel hydrotalcite prepared in example 1 before and after alkali-sulfur composite treatment, wherein (a) is before treatment and (b) is after treatment;
FIG. 3 is a constant current charge and discharge curve diagram of the cobalt-chromium-nickel hydrotalcite electrode material before and after the alkali-sulfur composite treatment prepared in example 1 when the current density is 1A/g;
FIG. 4 is a line graph of specific capacities of cobalt-chromium-nickel hydrotalcite electrode materials before and after the alkali-sulfur composite treatment prepared in example 1 at different current densities;
FIG. 5 is the XRD patterns of cobalt-chromium-nickel hydrotalcite prepared in example 2 before and after the alkali-sulfur composite treatment;
FIG. 6 is SEM images of cobalt-chromium-nickel hydrotalcite prepared in example 2 before and after alkali-sulfur composite treatment, wherein (a) is before treatment and (b) is after treatment;
FIG. 7 is TEM images of Co-Cr-Ni hydrotalcite prepared in example 2 before and after alkali-sulfur complex treatment, wherein (a) is before treatment and (b) is after treatment;
FIG. 8 is a constant current charge/discharge curve diagram of the Co-Cr-Ni hydrotalcite electrode material prepared in example 2 before and after the alkali-sulfur composite treatment, when the current density is 1A/g;
FIG. 9 is a line graph of specific capacities of cobalt chromium nickel hydrotalcite electrode materials before and after the alkali-sulfur composite treatment prepared in example 2 at different current densities;
FIG. 10 is the XRD patterns of cobalt-chromium-nickel hydrotalcite prepared in example 3 before and after the alkali-sulfur composite treatment;
FIG. 11 is an SEM image of cobalt-chromium-nickel hydrotalcite prepared in example 3 before and after an alkali-sulfur complex treatment, wherein (a) is before treatment and (b) is after treatment;
FIG. 12 is a constant current charge/discharge curve diagram of the Co-Cr-Ni hydrotalcite electrode material before and after the alkali-sulfur composite treatment prepared in example 3 when the current density is 1A/g;
FIG. 13 is a plot of specific capacity of cobalt chromium nickel hydrotalcite electrode materials prepared in example 3 before and after alkali-sulfur composite treatment at different current densities;
FIG. 14 is a flow chart of the method for alkali-sulfur composite treatment of cobalt-chromium-nickel hydrotalcite supercapacitor electrode material.
Detailed Description
Other aspects, features and advantages of the present invention will become apparent from the following detailed description, taken in conjunction with the accompanying drawings, which form a part of this specification, and which illustrate, by way of example, the principles of the invention. In the referenced drawings, the same or similar components in different drawings are denoted by the same reference numerals.
Example 1
As shown in fig. 14, the method for preparing a supercapacitor material by alkali-sulfur composite treatment of cobalt-chromium-nickel hydrotalcite according to the present invention comprises the following steps:
1. preparing a reaction solution: preparing an 80ml aqueous solution from 38mmol/L cobalt metal salt solution, 19mmol/L chromium metal salt solution, 13mmol/L nickel metal salt solution and 50mmol/L precipitator, and stirring uniformly by using a magnetic stirrer;
2. hydrothermal reaction: putting the prepared solution into a reaction kettle, heating the reaction kettle to 160 ℃ under normal pressure, and preserving heat for 4 hours;
3. and (3) post-treatment: and (3) cleaning and filtering the solution in the reaction kettle by adopting water and ethanol for multiple times to obtain a filter cake, putting the filter cake into a drying oven for drying at 60 ℃, and then grinding the filter cake into powder to obtain the cobalt-chromium-nickel hydrotalcite powder.
4. Preparing an alkali and sulfur composite solution: mixing 1mol/L NaOH solution and 2mol/L Na2Mixing the S solution according to the ratio of 2:1, and stirring the mixture uniformly by using a magnetic stirrer;
5. and (3) adding 0.6g of cobalt chromium nickel hydrotalcite powder into the alkali and sulfur composite solution, stirring for 24 hours at normal temperature and normal pressure, filtering, drying and grinding to obtain the cobalt chromium nickel hydrotalcite powder subjected to alkali and sulfur composite treatment.
FIG. 1 is an XRD pattern of cobalt-chromium-nickel hydrotalcite obtained in example 1 before and after the alkali-sulfur complex treatment. Corresponding to PDF card (JCPDS #46-0605), the 2 theta angles corresponding to characteristic diffraction peaks of (003), (006), (101), (012), (110) and (113) crystal planes are respectively 11.5 degrees, 23.2 degrees, 34.1 degrees, 39.0 degrees, 59.7 degrees and 61.1 degrees, and the typical layered structure is obtained before and after the processing. The disappearance of the characteristic peak of the (012) plane and the decrease of the diffraction intensity of the diffraction peaks of the (003) and (006) planes after the alkali and sulfur compound treatment indicate that the crystallinity of the material after the treatment is decreased.
Fig. 2 is an SEM image of the cobalt chromium nickel hydrotalcite material obtained in example 1 before and after the alkali-sulfur composite treatment at 30000 times magnification. It can be seen from the figure that after the alkali-sulfur composite treatment of example 1, the cobalt-chromium-nickel hydrotalcite has rough surface and generates granular structure, which indicates that amorphous sulfide is formed, and the generation of sulfide can improve the conductivity of the material.
The capacitive energy of cobalt chromium nickel hydrotalcite material before and after the alkali and sulfur composite treatment was prepared and tested using the Shanghai Chenghua CHI660E electrochemical workstation. In a three-electrode system, materials before and after alkali and sulfur composite treatment are used as working electrodes, a platinum sheet is used as a counter electrode, Hg/HgO is used as a reference electrode of the three-electrode system, electrochemical performance tests are carried out in a KOH solution of 1mol/L, and FIG. 3 shows that the specific capacitance of the treated materials is increased from 955.1F/g to 1164.9F/g compared with the materials before treatment according to a constant current charge-discharge curve of the cobalt-chromium-nickel hydrotalcite materials before and after the alkali and sulfur composite treatment obtained in example 1 when the current density is 1A/g. Fig. 4 is a specific capacity line graph of the cobalt-chromium-nickel hydrotalcite material before and after the alkali-sulfur composite treatment obtained in example 1 under different current densities, and when the current density is 20A/g, the rate performance after the alkali-sulfur composite treatment is increased from 48.81% to 49.43%.
Example 2
wherein, step 4, preparing alkali and sulfur composite solution: 2mol/L NaOH solution and 2mol/L Na2Mixing the S solution according to the ratio of 2:1, and stirring the mixture uniformly by using a magnetic stirrer;
FIG. 5 is an XRD pattern of cobalt-chromium-nickel hydrotalcite obtained in example 2 before and after the alkali-sulfur complex treatment. Corresponding to PDF card (JCPDS #46-0605), the 2 theta angles corresponding to the characteristic diffraction peaks of the (003), (006), (101), (012), (110) and (113) crystal planes are respectively 11.5 degrees, 23.2 degrees, 34.1 degrees, 39.0 degrees, 59.7 degrees and 61.1 degrees, and the layered structure is not changed before and after the treatment. The disappearance of the characteristic peak of the (012) plane and the decrease of the diffraction intensity of the diffraction peaks of the (003) and (006) planes after the alkali and sulfur compound treatment indicate that the crystallinity of the material after the treatment is decreased.
Fig. 6 is an SEM image of the cobalt chromium nickel hydrotalcite material obtained in example 2 before and after the alkali-sulfur composite treatment at 30000 times magnification. It can be seen from the figure that after the alkali and sulfur compound treatment of example 2, the cobalt-chromium-nickel hydrotalcite has a granular structure of 100nm, which indicates that amorphous sulfide is formed, and the generation of sulfide can improve the conductivity of the material.
FIG. 7 is a TEM image of cobalt-chromium-nickel hydrotalcite obtained in example 2 before and after the alkali-sulfur complex treatment. The material before the alkali and sulfur composite treatment has obvious lattice stripes which are clear and consistent in orientation, and the result shows that the cobalt-chromium-nickel hydrotalcite material has a uniform structure, good crystallinity and a stable structure. The material part area still presents obvious lattice stripes after the alkali and sulfur composite treatment. Wherein the presence of the lattice defect promotes the rate of ion diffusion due to the presence of significant lattice defects as a result of the etching action. While the sulfuration treatment generates amorphous sulfide which presents an amorphous structure, and the existence of the amorphous structure is one of the reasons for improving the specific capacity and having excellent rate capability.
The electrochemical performance test method of this example is the same as that of example 1, fig. 8 is a constant current charge and discharge curve of the cobalt-chromium-nickel hydrotalcite material obtained in example 2 before and after the alkali-sulfur composite treatment when the current density is 1A/g, and the specific capacitance of the treated material is increased from 955.1F/g to 1501.03F/g compared with the material before the treatment. Fig. 9 is a specific capacity line graph of the cobalt-chromium-nickel hydrotalcite material before and after the alkali-sulfur composite treatment obtained in example 2 under different current densities, and when the current density is 20A/g, the rate performance after the alkali-sulfur composite treatment is increased from 48.81% to 64.63%.
Table 1 shows the content of Co, Cr, Ni and hydrotalcite under etching and sulfurization conditions obtained in example 2. The etching effect reduces the content of Cr element, and the sulfurization effect increases the content of S element.
TABLE 1
Example 3
wherein, step 4, preparing alkali and sulfur composite solution: 4mol/L NaOH solution and 2mol/L Na2Mixing the S solution according to the ratio of 2:1, and stirring the mixture uniformly by using a magnetic stirrer;
FIG. 10 is an XRD pattern of cobalt-chromium-nickel hydrotalcite obtained in example 3 before and after the alkali-sulfur complex treatment. Corresponding to the PDF card (JCPDS #46-0605), the card has a typical layered structure before and after processing. The disappearance of the characteristic peak of the (012) plane and the decrease of the diffraction intensity of the diffraction peaks of the (003) and (006) planes after the alkali and sulfur compound treatment indicate that the crystallinity of the material after the treatment is decreased.
Fig. 11 is an SEM image of the cobalt chromium nickel hydrotalcite material obtained in example 3 before and after the alkali-sulfur composite treatment at 30000 times magnification. It can be seen from the figure that after the alkali and sulfur compound treatment of example 3, the cobalt-chromium-nickel hydrotalcite has rough surface and generates granular structure, which indicates that amorphous sulfide is formed, and the generation of sulfide can improve the conductivity of the material.
The electrochemical performance test method of this example is the same as that of example 1. FIG. 12 is a constant current charge/discharge curve of the cobalt chromium nickel hydrotalcite material before and after the alkali-sulfur composite treatment obtained in example 3, when the current density is 1A/g, the specific capacitance of the treated material is increased from 955.1F/g to 985.34F/g compared with the material before the treatment. Fig. 4 is a specific capacity line graph of the cobalt-chromium-nickel hydrotalcite material before and after the alkali-sulfur composite treatment obtained in example 3 under different current densities, and when the current density is 20A/g, the rate capability after the alkali-sulfur composite treatment is increased from 48.81% to 54.94%.
Firstly, preparing a cobalt-chromium-nickel hydrotalcite precursor by a hydrothermal method, and then adding NaOH solution and Na into cobalt-chromium-nickel hydrotalcite powder2The S solution is mixed according to a certain proportion to form a uniform alkali-sulfur composite solution, and the uniform alkali-sulfur composite solution is stirred at normal temperature and normal pressure to realize the etching and vulcanization of the cobalt-chromium-nickel hydrotalcite. In the process of alkali and sulfur composite treatment, Cr is caused by etching action3+The crystal lattice defect is formed by dissolving NaOH, the ion diffusion rate is promoted, and the cobalt-chromium-nickel hydrotalcite generates amorphous sulfide by the sulfuration action, and the sulfide has the advantages of high conductivity and high specific capacity. The preparation method is simple and low in cost, the prepared supercapacitor material has excellent electrochemical performance, and the optimal specific capacitance after the alkali-sulfur composite treatment is increased from 955.1F/g to 1501.3F/g compared with untreated cobalt-chromium-nickel hydrotalcite within 0-0.7V of potential and under the current density of 1A/g. The rate capability is increased from 48.81% to 64.63% at a current density of 20A/g.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
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