CN110120306B - Co-Mo-O-S spherical flower cluster structure composite material and preparation method and application thereof - Google Patents
Co-Mo-O-S spherical flower cluster structure composite material and preparation method and application thereof Download PDFInfo
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- CN110120306B CN110120306B CN201910438330.1A CN201910438330A CN110120306B CN 110120306 B CN110120306 B CN 110120306B CN 201910438330 A CN201910438330 A CN 201910438330A CN 110120306 B CN110120306 B CN 110120306B
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- H—ELECTRICITY
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a Co-Mo-O-S spherical flower cluster structure composite material, the microstructure of which is a spherical flower cluster structure, a ball core is taken as a main body, and petals are fully grown on the ball core; the components of the spherical core are CoS and MoS2The petal is Mo8O23. The preparation method comprises the following steps: 1) preparing a Co-Mo-O precursor; 2) and preparing the Co-Mo-O-S spherical flower cluster composite material. The super capacitor electrode material is applied to charge and discharge in the range of 0-0.35V, and the specific capacitance is 1100-1200F/g when the discharge current density is 1A/g. The invention avoids introducing the carbon material with low specific capacitance, and comprises the following components: 1. only a hydrothermal method is needed, sintering carbonization is not needed, the preparation process is simple, and the energy consumption is low; 2. has high specific capacitance. Meanwhile, through vulcanization operation, a spherical flower cluster structure is realized, and the circulation stability of the material is greatly improved.
Description
Technical Field
The invention relates to the technical field of sulfide composite material preparation, in particular to a Co-Mo-O-S spherical flower cluster structure composite material and a preparation method and application thereof.
Background
As a high-efficiency energy storage device with bright prospect, the super capacitor has attracted extensive research interest of researchers due to the advantages of high power density, fast charge-discharge rate, long cycle life and the like. The core of the super capacitor, namely the electrode material, can directly influence the main performance index of the super capacitor, and in view of the present, the main direction of research on the super capacitor is to find a more ideal and low-cost electrode material.
The electrode material of the double electric layer capacitor, such as a carbon material, has the characteristic of good stability, but cannot meet the application requirement due to lower specific capacitance; in contrast, faraday capacitive electrode materials, such as transition metal oxides and transition metal sulfides, have much higher specific capacitance performance than double layer capacitive materials.
However, in the prior art, when the faraday capacitance electrode material is prepared, a single metal element is adopted as the faraday capacitance electrode material, and the problem that the material microstructure is unstable, which results in poor cyclicity of the supercapacitor material, exists. In order to solve this problem, the prior art adopts a method of loading a transition metal oxide or a transition metal sulfide on a carbon material having a stable microstructure.
In the prior art of transition metal oxides, Pan super et al (Hi-Tech Fiber & Application, 2017, stage 01, ISSN: 1007-9815) combines modified metal oxide nanoparticles with graphene to obtain a graphene-coated metal oxide material for a supercapacitor. The specific capacitance of the material is only 411F/g when the discharge current density is 1A/g; after 3000 cycles, the cycle life is only kept at 70% of the original capacitance; after the hydrothermal reaction, the material is sintered to prepare the final sample.
In the prior art of transition metal sulfides, Gaoyang et al (research on preparation of multi-element metal sulfide electrode material and performance of supercapacitor thereof, Zhengzhou university, classification number: TM 53) synthesizes a large amount of CoS with three-dimensional hierarchical structure by taking Co functional coordination compound as precursor and adopting simple solvothermal reaction1.097Micro-flowers of rice, CoS finally obtained1.097The micro-flower is used as the electrode material of the super capacitor. The electrochemical performance result shows that the CoS of the single metal1.097The specific capacity of the micro-flower is only 533F/g, and the multiplying power is 84%. The specific capacitance and the cycle performance are both at a low level, therefore, the technology is to CoS1.097The micro-popcorn is loaded on the carbon material graphene oxide to further improve the material performance, and finally the specific capacitance of 810F/g and the rate performance of up to 90% are obtained.
Also, DyeJer et al (MoS of different morphology2And MoS2Application of composite material in super capacitor (Lanzhou university, classification number TM53, TB 33) only preparing transition metal sulfide MoS2As an electrode material of a super capacitor, MoS is only realized at a current density of 0.5A/g2Has a specific capacity of 145F/g, and the measured capacitance is 65% of the initial capacitance after 1000 cycles. The solution provided by the prior art is also compounded with carbon fiber carbon material, the specific capacitance is improved to 400F/g, and the rate is improved to 74% from 65%.
As can be seen from the analysis of the above prior art, the problem of cycle stability cannot be solved only by using a single transition metal oxide or transition metal sulfide, and the problem must be solved by loading a carbon material.
The prior art methods of loading carbon materials all have the following technical problems:
1. although the carbon material can improve the stability of the supercapacitor, the specific capacitance provided by the supercapacitor is small, and the effect of improving the stability of the supercapacitor is realized by adding a large amount of carbon material, so that the integral specific capacitance of the supercapacitor material is inevitably reduced greatly;
2. the preparation process of the carbon material requires (after hydrothermal reaction) sintering and carbonizing the carbon-containing material to prepare the final electrode material, and obviously has the technical problems of high energy consumption and complex preparation process.
Disclosure of Invention
The invention aims to provide a Co-Mo-O-S spherical flower cluster structure composite material and a preparation method thereof.
The method is a method for compounding various high-specific-capacitance Faraday capacitance electrode materials, transition metal oxides and transition metal sulfides to replace carbon material loading. The method does not need a composite carbon material, so that the sintering and carbonizing processes are reduced, and the technical effects of simplifying the preparation process and reducing the energy consumption are realized; meanwhile, as the composite materials are all Faraday capacitance electrode materials with high specific capacitance, the specific capacitance of the super capacitor can be improved under the condition that the cycle performance of the super capacitor is maintained and improved without carbon material loading.
However, it is confirmed by the contents of the embodiments of the present invention that the improvement and improvement of the electrochemical performance cannot be achieved by simply compounding two transition metal oxides and transition metal sulfides in the prior art. Therefore, the bimetallic synergistic effect generated between transition metals is needed to achieve the above purpose.
The prior art adopts a multi-metal sulfide coprecipitation method, and has the problems that the precipitation rate of two or more inorganic salts cannot be controlled, so that the prepared material particles are not uniform, the appearance is not controllable, and the heterogeneity is realized. In order to overcome the technical problems, the invention adopts a two-step hydrothermal method, effectively controls the particle size and the micro morphology of the material, obtains a spherical flower cluster structure, and improves the specific capacitance and the cycling stability of the material.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that:
Co-Mo-O-S spherical flower cluster structure composite material made of Co (NO)3)2·6H2O、(NH4)6Mo7O24·4H2O、CO(NH2)2、NH4F and soluble sulfide are used as starting materials and are prepared by hydrothermal reaction. The microstructure is a spherical cluster structure, a ball core is taken as a main body, and petals grow on the ball core; the components of the spherical core are CoS and MoS2The petal is Mo8O23。
The preparation method of the Co-Mo-O-S spherical flower cluster structure composite material comprises the following steps:
1) preparation of Co-Mo-O precursor, Co (NO)3)2·6H2O、(NH4)6Mo7O24·4H2O、CO(NH2)2、NH4F is weighed according to the weight ratio of (2-4) to 0.4:6:4Dissolving in water, magnetically stirring for 15-25min, transferring the solution into a high-pressure kettle, keeping at 120-140 ℃ for 4-6 h, cooling to room temperature, performing suction filtration, and drying to obtain a Co-Mo-O precursor;
2) the preparation method comprises the steps of firstly weighing a Co-Mo-O precursor and a soluble sulfide according to the mass ratio of 3 (10-30) of the Co-Mo-O precursor to the soluble sulfide, dissolving the Co-Mo-O precursor in water, carrying out ultrasonic treatment, then pouring a soluble sulfide aqueous solution, transferring the obtained mixed solution into a high-pressure kettle, keeping the mixed solution at the temperature of 100 ℃ and 120 ℃ for 11-13 h, cooling to room temperature, carrying out suction filtration and drying to obtain the Co-Mo-O-S composite material.
The application of the Co-Mo-O-S spherical flower cluster structure composite material as the electrode material of the super capacitor is characterized in that: the discharge is carried out in the range of 0-0.35V, and the specific capacitance is 1100-1200F/g when the discharge current density is 1A/g.
The Co-Mo-O-S spherical flower cluster structure composite material obtained by the invention is detected by experiments, and the result is as follows:
in order to prove the size and the particle size distribution of the Co-Mo-O-S spherical flower cluster structure composite material, the particle size of the material is 2-5 mu m through the test of a scanning electron microscope.
In order to prove the structural characteristics of the Co-Mo-O-S spherical flower cluster structure composite material, the structure of the material is a spherical flower cluster structure through transmission electron microscope testing.
The electrochemical performance test of the Co-Mo-O-S spherical flower cluster structure composite material detects that the Co-Mo-O-S spherical flower cluster structure composite material is charged and discharged within the range of 0-0.35V, and when the discharge current density is 1A/g, the specific capacitance range of the electrode of the Co-Mo-O-S spherical flower cluster structure composite material super capacitor is 1100-1200F/g, which shows that the Co-Mo-O-S spherical flower cluster structure composite material has good super capacitance performance.
Compared with the prior art, the Co-Mo-O-S spherical flower cluster structure composite material has the following advantages:
1. the invention adopts Co (NO)3)2·6H2O、(NH4)6Mo7O24·4H2O、CO(NH2)2、NH4F and soluble sulfide are used as reaction reagents to prepare the Co-Mo-O-S spherical flower cluster structure composite materialThe effect of improving the stability of the super capacitor is realized under the condition that no carbon material is added, and the specific capacitance is 1100-1200F/g;
2, synthesizing the Co-Mo-O-S spherical flower cluster structure composite material by adopting a two-step hydrothermal method, wherein the oxide is obtained in the first step of hydrothermal method, and the sulfide is obtained in the second step of hydrothermal method, so that compared with the one-step hydrothermal method, the particle size and the micro morphology of the material can be effectively controlled, the spherical flower cluster structure is obtained, and the specific capacitance and the cycling stability of the material are improved; the obtained material does not need sintering carbonization, and the energy consumption is low;
3. the Co-Mo-O-S spherical flower cluster structure composite material has an easily understood treatment process and is suitable for mass preparation.
Therefore, the invention has wide application prospect in the field of super capacitor materials.
Drawings
FIG. 1 is a scanning electron microscope image of a Co-Mo-O-S spherical floral cluster structure composite material with a sulfur ion concentration of 0.2M prepared in example 1;
FIG. 2 is a scanning electron microscope image of a Co-Mo-O-S spherical floral cluster structure composite material prepared in comparative example 2 and having a sulfide ion concentration of 0.3M;
FIG. 3 is a scanning electron microscope image of a Co-Mo-O-S spherical floral cluster structure composite material having a sulfide ion concentration of 0.4M prepared in comparative example 2;
FIG. 4 is a transmission electron microscope image of a Co-Mo-O-S spherical floral structure composite prepared in example 1;
FIG. 5 is a graph showing the discharge curves of the Co-Mo-O-S spherical floral cluster composite prepared in example 1 and the Co-Ni-O-S composite prepared in comparative example 1;
FIG. 6 is a graph showing discharge curves of the Co-Mo-O-S spherical floral cluster composite having a sulfide ion concentration of 0.2M prepared in example 1 and the Co-Mo-O-S composite having a sulfide ion concentration of 0.3M and the Co-Mo-O-S composite having a sulfide ion concentration of 0.4M prepared in comparative example 2;
FIG. 7 is a graph showing the discharge curves of the Co-Mo-O-S spherical floral cluster composite of example 1 prepared by two hydrothermal steps and the Co-Mo-O-S spherical floral cluster composite of comparative example 3 prepared by one hydrothermal step;
FIG. 8 is an XRD of the Co-Mo-O precursor and Co-Mo-O-S spherical floral cluster composite prepared in example 1;
FIG. 9 is a cycle life curve for the Co-Mo-O-S spherical floral cluster composite prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings, which are given by way of examples, but are not intended to limit the present invention.
Example 1
A preparation method of a Co-Mo-O-S spherical flower cluster-shaped composite material comprises the following steps:
step 1) preparation of Co-Mo-O precursor, Co (NO)3)2·6H2O、(NH4)6Mo7O24·4H2O、CO(NH2)2、NH4F is weighed according to the mass ratio of 2:0.4:6:4 and then dissolved in water, the mixture is magnetically stirred for 20 min, the obtained solution is transferred into a high-pressure kettle and kept at 130 ℃ for 5 h, the mixture is cooled to room temperature, and a Co-Mo-O precursor is obtained through suction filtration and drying;
step 2) preparation of Co-Mo-O-S spherical floral cluster composite material, 0.1g of Co-Mo-O precursor is taken to be dissolved in water and subjected to ultrasonic treatment, and then 30ml of Na with the sulfur ion concentration of 0.2M is poured2And (3) transferring the mixed solution into a high-pressure kettle, keeping the temperature at 110 ℃ for 12 h, cooling to room temperature, carrying out suction filtration, and drying to obtain the Co-Mo-O-S composite material.
In order to prove the size and the particle size distribution of the Co-Mo-O-S spherical bouquet structure composite material, the particle size of the material is 2-5 μm as shown in figure 1 through a scanning electron microscope test.
In order to prove the structural characteristics of the Co-Mo-O-S spherical bouquet structure composite material, the structure of the material is a spherical bouquet structure as shown in FIG. 4 through a transmission electron microscope test.
The electrochemical performance test method of the Co-Mo-O-S spherical flower cluster-shaped composite material comprises the following steps: weighing 0.008 g of Co-Mo-O-S composite material, 0.001 g of acetylene black and 0.001 g of polytetrafluoroethylene micro powder, placing the materials in a small agate grinding bowl, and adding 0.5 mL of ethanol for grinding; and pressing the ground sample with a foamed nickel current collector with the thickness of 1 mm under the pressure of 10 kPa, drying in air at room temperature, cutting into 2 cm multiplied by 2 cm to prepare the electrode of the super capacitor, and testing the specific capacitance of the electrode.
As shown in fig. 5, the following results were obtained: the super capacitor is charged and discharged within the range of 0-0.35V, and the specific capacitance of the electrode of the Co-Mo-O-S spherical flower cluster composite material super capacitor is 1142F/g when the discharge current density is 1A/g.
Comparative example 1
In order to study the influence of the bimetallic synergistic effect generated between transition metals on the material performance, a Co-Ni-O-S composite material was prepared, and the steps not specifically described in the specific steps were the same as the preparation method of the Co-Mo-O-S composite material described in this example.
The difference lies in that: step 1 is to add (NH)4)6Mo7O24·4H2Replacement of O by Ni (NO)3)2·6H2And preparing O.
The obtained Co-Ni-O-S composite material was subjected to electrochemical tests in the same manner as in example 1, and the results of the tests are shown in FIG. 5, in which the composite material was charged and discharged at a voltage of 0 to 0.35V and had a specific capacitance of 340F/g at a discharge current density of 1A/g.
Therefore, under the same current density, the discharge time of the Co-Mo-O-S electrode material is obviously longer than that of the Co-Ni-O-S electrode material, and the discharge time is improved by more than 4 times, which shows that the specific capacitance of the Co-Mo-O-S electrode material is obviously improved compared with that of the Co-Ni-O-S electrode material, and shows that the Co-Mo-O-S composite material has good super-capacitance performance.
Comparative example 2
In order to study the influence of the micro-morphology on the performance of the Co-Mo-O-S composite material, namely the influence of the experimental process on the performance of the material, the raw materials are controlled to be completely the same, and the Co-Mo-O-S composite material with different sulfide ion concentrations is prepared only by changing the parameters of the experimental process, wherein the steps which are not particularly described in the specific steps are the same as the preparation method of the Co-Mo-O-S composite material with the sulfide ion concentration of 0.2M in the embodiment.
The difference lies in that: the sulfur ion concentration in step 3 was changed from 0.2M to 0.3M and 0.4M.
The micro-morphology of the Co-Mo-O-S composite material with the sulfide ion concentration of 0.3M and the sulfur ion concentration of 0.4M prepared in the comparative example is shown in figures 2 and 3 through a scanning electron microscope test, and the experimental result shows that the micro-morphology of the material obtained in the comparative example is large-particle-shaped instead of a spherical cluster structure.
The electrochemical performance test method was the same as that of example 1, and the results are shown in FIG. 6, where the specific capacitances of the obtained Co-Mo-O-S composite materials with large particle shapes (non-spherical flower cluster structures) and sulfur ion concentrations of 0.3M and 0.4M were 733F/g and 210F/g, respectively, at a discharge current density of 1A/g.
Therefore, the micro-morphology of the material has obvious influence on the performance, and the specific capacitance of the spherical flower cluster structure composite material is 1.5 times and 5 times of that of the large-particle composite material with the sulfide ion concentration of 0.3M and that of the large-particle composite material with the sulfide ion concentration of 0.4M respectively, which shows that the micro-morphology of the spherical flower cluster structure directly obtains the technical effect of obviously improving the capacitance performance of the composite material.
Therefore, the composite material can realize excellent electrochemical performance only by being made into a spherical flower cluster shape by the process technology provided by the invention.
Comparative example 3
In order to study the influence of the hydrothermal method on the performance of the Co-Mo-O-S spherical flower cluster composite material by adopting a one-step method or a two-step method, namely the influence of an experimental process on the performance of the material, the raw materials are controlled to be completely the same, and only experimental process parameters are changed, so that the Co-Mo-O-S composite material obtained by one-step hydrothermal method is prepared.
The difference lies in that: said step 3 is eliminated and 30ml of Na is added2The aqueous solution of S is directly poured into the solution prepared in step 1.
XRD of the Co-Mo-O-S spherical floral cluster structure composite material prepared by the two-step hydrothermal method is shown in FIG. 8, and it can be seen that MoO and CoO are obtained from the Co-Mo-O precursor prepared by the first-step hydrothermal method, and that MoO and CoO are obtained from the Co-Mo-O precursor and Na2MoS is obtained from Co-Mo-O-S composite material prepared by S twice hydrothermal2And CoS, which is not achievable in a single step hydrothermal preparation of Co-Mo-O-S composites.
The Co-Mo-O-S composite material hydrothermally prepared in one step in the comparative example was subjected to electrochemical tests in the same manner as in example 1, and the results of the tests are shown in FIG. 7, in which the composite material was charged and discharged at a voltage of 0 to 0.35V and had a specific capacitance of 302F/g at a discharge current density of 1A/g.
Therefore, the material prepared by the two-step hydrothermal method has obvious influence on the performance, the specific capacitance of the spherical flower cluster structure composite material is 3.5 times that of the Co-Mo-O-S composite material prepared by the one-step hydrothermal method, the performance of the Co-Mo-O-S composite material with the spherical flower cluster structure is obviously improved, and the Co-Mo-O-S composite material has good super-capacitance performance.
Claims (3)
1. A Co-Mo-O-S spherical flower cluster structure composite material is characterized in that: the microstructure is a spherical cluster structure, a ball core is taken as a main body, and petals grow on the ball core; the components of the spherical core are CoS and MoS2The petal is Mo8O23(ii) a With Co (NO)3)2·6H2O、(NH4)6Mo7O24·4H2O、CO(NH2)2、NH4F and soluble sulfide are used as initial raw materials and are prepared by hydrothermal reaction, wherein the soluble sulfide is Na2S。
2. The method for preparing a Co-Mo-O-S spherical bouquet structure composite material according to claim 1, characterized by comprising the steps of:
step 1) preparation of Co-Mo-O precursor, weighing Co (NO) according to a certain mass ratio3)2·6H2O、(NH4)6Mo7O24·4H2O、CO(NH2)2、NH4Dissolving F in water, magnetically stirring for 15-25min, transferring the solution into a high-pressure kettle, keeping the temperature at 120-140 ℃ for 4-6 h, cooling to room temperature, performing suction filtration, and drying to obtain a Co-Mo-O precursor;
co (NO) used in said step 1)3)2·6H2O、(NH4)6Mo7O24·4H2O、CO(NH2)2、NH4The mass ratio of F is (2-4) 0.4:6: 4;
step 2) preparing a Co-Mo-O-S spherical flower cluster composite material, weighing a Co-Mo-O precursor according to a certain substance amount ratio, dissolving the Co-Mo-O precursor in water, performing ultrasonic treatment, pouring a soluble sulfide aqueous solution to obtain a mixed solution, transferring the mixed solution into a high-pressure kettle, keeping the mixed solution at the temperature of 100 ℃ and 120 ℃ for 11-13 h, cooling to room temperature, performing suction filtration and drying to obtain the Co-Mo-O-S composite material;
the mass ratio of the Co-Mo-O precursor and the soluble sulfide used in the step 2) is 3 (10-30); the concentration of the sulfide ions in the soluble sulfide aqueous solution in the step 2) is 0.1-0.2M.
3. The application of the Co-Mo-O-S spherical flower cluster structure composite material as a supercapacitor electrode material according to claim 1, wherein the Co-Mo-O-S spherical flower cluster structure composite material is characterized in that: the discharge is carried out in the range of 0-0.35V, and the specific capacitance is 1100-1200F/g when the discharge current density is 1A/g.
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