CN109786117B - Carbon nano tube-cobaltosic sulfide composite material and preparation method and application thereof - Google Patents
Carbon nano tube-cobaltosic sulfide composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a carbon nano tube-cobaltosic sulfide nickel composite material and a preparation method and application thereof, and the preparation method comprises the following steps: (1) ultrasonically dispersing a carbon nano tube, ammonia water, ethyl orthosilicate and surfactant in a mixed solution of ethanol and water, stirring for reaction, and filtering and drying the obtained powder; (2) dispersing the powder in the last step, nickel nitrate, cobalt nitrate and an alkaline environment promoter in deionized water, carrying out hydrothermal reaction, and then carrying out suction filtration, cleaning and drying on a cooled product; (3) and dispersing the powder obtained in the last step in a sodium sulfide aqueous solution, and carrying out hydrothermal reaction to finally obtain the carbon nano tube-cobaltosic sulfide composite material. The invention has the beneficial effects that: the capacity and the cycling stability of the material are improved.
Description
Technical Field
The invention relates to the technical field of material chemistry, in particular to a carbon nano tube-cobaltosic sulfide composite material and a preparation method and application thereof.
Background
The cobaltosic nickel sulfide has the characteristics of high pseudo capacitance capacity of the super capacitor, rich element sources, high conductivity relative to nickel sulfide and cobalt sulfide, and the like, and is a very potential super capacitor material. But the conductivity of the super capacitor still cannot meet the use requirement of the super capacitor on high current density, the capacity loss is large under high power, and the rate capability is poor. The carbon nano tube has good crystallinity, excellent mechanical and electrical properties and high specific surface area, and can provide an ideal conductive network for other materials. The active material and the carbon nano tube are compounded to form a carbon nano tube network to provide an electronic channel for the active material, so that the conductivity of the cobaltosic sulfide nickel can be effectively improved, the rapid ion adsorption, desorption and transmission between the cobaltosic sulfide nickel and the electrolyte are facilitated, and the performance of the material under high-rate current density is remarkably improved. In addition, the carbon nano tube has high specific surface area, and the specific surface area of the carbon nano tube can be obviously improved by carrying out coating type compounding on the carbon nano tube and the cobaltosic sulfide, so that more reaction active sites are provided, and the capacity of the material is improved.
Disclosure of Invention
The invention aims to provide a carbon nano tube-cobaltosic sulfide composite material, a preparation method and application thereof, aiming at the technical defects in the prior art.
The technical scheme adopted for realizing the purpose of the invention is as follows:
the invention relates to a preparation method of a carbon nano tube-cobaltosic sulfide composite material, which comprises the following steps:
step 2, adding the carbon nano tube-cobalt nickel silicate composite material prepared in the step 1 into a mixed solvent of ethanol and deionized water, wherein the concentration of the carbon nano tube-cobalt nickel silicate composite material is 0.1g L-1～0.4g L-1Wherein the volume ratio of the ethanol to the deionized water is 1: (2-4), then adding sodium sulfide, wherein the mass ratio of the sodium sulfide to the carbon nano tube-cobalt nickel silicate composite material is (4-8): 1, after even dispersion, carrying out hydrothermal reaction for 10-15h at the temperature of 100-200 ℃, finally centrifuging and cleaning the obtained product, and freeze-drying to obtain the carbon nano tube-tetrasulfideA nickel cobalt composite material.
Preferably, the mass ratio of the alkaline environment promoter to the carbon nanotube-silicon oxide composite material in the step 1 is (1-2): (0.02-0.04), the Ni (NO)3)2The mass ratio of the carbon nano tube to the silicon oxide composite material is 1: (1.6-2.0), Co (NO)3)2The mass ratio of the carbon nano tube to the silicon oxide composite material is 1: (0.8-1.0).
Preferably, the preparation method of the carbon nanotube-silicon oxide composite material in the step 1 is as follows: dissolving a surfactant in a mixed solution of deionized water and ethanol, wherein the concentration of the surfactant is 1-2 gL-1Wherein the volume ratio of the deionized water to the ethanol is 1: (3-5), then adding ammonia water and hydroxylated carbon nanotube powder, wherein: the adding amount of ammonia water is 0.5-2% of the volume of the mixed solution, and the concentration of the carbon nano tube in the mixed solution is 0.5-0.8 g L-1And after uniform dispersion, dropwise adding Tetraethoxysilane (TEOS), wherein the adding amount of TEOS is 0.5-2% of the volume of the mixed solution, stirring and reacting for 5-10 h, then carrying out suction filtration and cleaning on the product, and drying for 10-15h at the temperature of 40-80 ℃ to obtain the carbon nano tube-silicon oxide composite material.
Preferably, the surfactant is cetyl trimethyl ammonium bromide, stearyl trimethyl ammonium bromide or stearyl trimethyl ammonium chloride.
Preferably, the alkaline environment promoter in step 1 is urea or ammonia water.
In another aspect of the present invention, the carbon nanotube-cobaltosic sulfide composite material is formed by carbon nanotubes and clustered or nanocrystalline cobaltosic sulfide coated on the surface of the carbon nanotubes to form a coaxial cable structure, and is prepared according to the following method:
step 2, adding the carbon nano tube-cobalt nickel silicate composite material prepared in the step 1 into a mixed solvent of ethanol and deionized water, wherein the concentration of the carbon nano tube-cobalt nickel silicate composite material is 0.1g L-1～0.4g L-1Wherein the volume ratio of the ethanol to the deionized water is 1: (2-4), then adding sodium sulfide, wherein the mass ratio of the sodium sulfide to the carbon nano tube-cobalt nickel silicate composite material is (4-8): 1, after uniform dispersion, carrying out hydrothermal reaction for 10-15h at the temperature of 100-200 ℃, and finally centrifuging and cleaning the obtained product, and freeze-drying to obtain the carbon nano tube-cobaltosic sulfide composite material.
Preferably, the mass ratio of the alkaline environment promoter to the carbon nanotube-silicon oxide composite material in the step 1 is (1-2): (0.02-0.04), the Ni (NO)3)2The mass ratio of the carbon nano tube to the silicon oxide composite material is 1: (1.6-2.0), Co (NO)3)2The mass ratio of the carbon nano tube to the silicon oxide composite material is 1: (0.8-1.0).
Preferably, the preparation method of the carbon nanotube-silicon oxide composite material in the step 1 is as follows: dissolving a surfactant in a mixed solution of deionized water and ethanol, wherein the concentration of the surfactant is 1-2 gL-1Wherein the volume ratio of the deionized water to the ethanol is 1: (3-5), then adding ammonia water and hydroxylated carbon nanotube powder, wherein: the adding amount of ammonia water is 0.5-2% of the volume of the mixed solution, and the concentration of the carbon nano tube in the mixed solution is 0.5-0.8 g L-1And after uniform dispersion, dropwise adding Tetraethoxysilane (TEOS), wherein the adding amount of TEOS is 0.5-2% of the volume of the mixed solution, stirring and reacting for 5-10 h, then carrying out suction filtration and cleaning on the product, and drying for 10-15h at the temperature of 40-80 ℃ to obtain the carbon nano tube-silicon oxide composite material.
Preferably, the surfactant is cetyl trimethyl ammonium bromide, stearyl trimethyl ammonium bromide or stearyl trimethyl ammonium chloride.
Preferably, the alkaline environment promoter in step 1 is urea or ammonia water.
Preferably, the carbon nanotube-cobaltosic sulfide composite material has a specific capacity of 400-700F/g at a current density of 1A/g.
In another aspect of the invention, the application of the carbon nanotube-cobaltosic sulfide composite material to an electrode material of a super capacitor is also included.
Preferably, the carbon nanotube-nickel tetrasulfide composite material is mixed with carbon black and Polytetrafluoroethylene (PTFE) according to the mass ratio of (5-10) to (1-2) and rolled or coated for preparing a supercapacitor material.
Compared with the prior art, the invention has the beneficial effects that:
1. the cobaltosic nickel sulfide prepared by the method has good supercapacitor performance, the synthesis process is simple and feasible, and the product is uniform.
2. The carbon nano tube-cobaltosic sulfide nickel composite material prepared by the method is composed of the carbon nano tube and cluster-shaped or nano crystal-shaped cobaltosic sulfide nickel coated on the surface of the carbon nano tube, the coating structure provides a large specific surface area for the material, the agglomeration is weakened, the structural stability is provided for the carbon nano tube framework, the carbon nano tube framework has good circulation stability, the carbon nano tube network provides an electron channel and an ion channel, the conductivity of the material is improved, the multiplying power performance of the material during charging and discharging under high current density is improved, and 84.3% of capacity can be still kept under 5A/g. A three-electrode test system is adopted to test the performance of the supercapacitor, the carbon nano tube-cobaltosic sulfide composite material has good cycle stability, and the cycle test is carried out at a sweep speed of 50mV/s, so that the material can still retain 80% of capacity after 1600 circles.
Drawings
FIG. 1 is an SEM image of the carbon nanotube-nickel cobaltosic sulfide composite obtained in example 1;
FIG. 2 is a TEM image of the carbon nanotube-nickel cobaltosic sulfide composite obtained in example 1;
FIG. 3 is a plot of cyclic voltammetry measurements at different scan rates for the carbon nanotube-nickel cobalttetrasulfide composite obtained in example 1;
FIG. 4 is a constant current charge-discharge curve of the carbon nanotube-cobaltosic sulfide composite obtained in example 1 at different charge-discharge rates;
FIG. 5 is a plot of the change in capacity calculated by cyclic voltammetry at a 50mV/s scan rate of 1600 cycle for the carbon nanotube-nickel tetrasulfide composite obtained in example 1;
fig. 6 is XRD patterns of the cobalt nickel silicate carbon nanotube composite and the carbon nanotube-cobaltosic sulfide composite obtained in example 1.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
(1) Dissolving 0.16g of hexadecyl trimethyl ammonium bromide in a mixed solution of 30ml of deionized water and 120ml of ethanol, adding 1.5ml of ammonia water and 0.1g of hydroxylated carbon nanotube powder, uniformly mixing in a beaker, and performing ultrasonic dispersion for 40 min. Then 1ml of Tetraethoxysilane (TEOS) is dripped in, and the mixture is stirred for 6 hours by magnetic force with the rotating speed of 60 r/min. Then, the product is filtered and cleaned, and dried for 12h at 60 ℃ to obtain CNT @ SiO2。
(2) And (3) adding 30mg of the powder material prepared in the previous step into a blue-covered glass bottle, adding 40ml of deionized water, and performing ultrasonic dispersion for 40 min. 1g of urea and 1ml of 0.1mol/L Ni (NO) are subsequently added3)2And 2ml of 0.1mol/L Co (NO)3)2Magnetically stirring the solution for 5min, sealing the bottle mouth, and carrying out hydrothermal reaction at 105 ℃ for 12 h. And then naturally cooling, carrying out suction filtration and cleaning on the obtained product, and drying at 60 ℃ for 12h to obtain the CNT @ NiCoSilicate.
(3) Taking 10mg of the powder prepared in the last step, adding 10ml of ethanol and 30ml of deionized water, adding certain 48mg of sodium sulfide, carrying out ultrasonic treatment for 40min, transferring the mixture into a 50ml hydrothermal kettle, and carrying out hydrothermal reaction for 12h at 160 ℃. And then centrifuging and cleaning the obtained product, and freeze-drying to obtain the product carbon nano tube-cobaltosic sulfide composite material.
X-ray diffraction analysis was performed on the cobalt nickel silicate carbon nanotube composite material and the carbon nanotube-cobaltosic sulfide composite material obtained in this example to obtain an image shown in fig. 6, which shows that the obtained material structure conforms to the standard card.
Scanning electron microscope analysis and transmission electron microscope analysis are performed on the carbon nanotube-cobaltosic sulfide composite material obtained in the present example, to obtain images as shown in fig. 1 and 2, and it can be seen from the figures that the obtained material has a coaxial cable coating structure.
The cyclic voltammetry detection of different multiplying powers is carried out on the sample, a curve as shown in figure 3 is obtained, and the graph shows that a pair of redox peaks appearing in the image accord with the characteristics of the cobaltosic sulfide nickel-nickel composite material.
The sample was subjected to chronopotentiometric measurements at different charge/discharge rates to obtain a curve as shown in FIG. 4, which shows that at a charge/discharge rate of 1A/g, the discharge time of the sample was 312s, and the corresponding capacitance value was 688F/g, while the capacitance value at 5A/g was 580F/g, which retained 84.3%.
The cyclic voltammetry cyclic life test is carried out on the sample for 1600 cycles to obtain a curve shown in fig. 5, and the graph shows that the material performance continuously decreases at a certain rate after the material is cycled for 1600 cycles, and finally 80% of the initial capacity is reserved, so that the cyclic stability is good.
Example 2
(1) Dissolving 0.2g of hexadecyl trimethyl ammonium bromide in a mixed solution of 30ml of deionized water and 120ml of ethanol, adding 1.5ml of ammonia water and 0.1g of hydroxylated carbon nanotube powder, uniformly mixing in a beaker, and performing ultrasonic dispersion for 40 min. Then 1ml of Tetraethoxysilane (TEOS) is dripped in, and the mixture is stirred for 6 hours by magnetic force with the rotating speed of 60 r/min. Then the product is filtered and washed, and dried for 12h at 60 ℃.
(2) And (3) adding 30mg of the powder material prepared in the previous step into a blue-covered glass bottle, adding 40ml of deionized water, and performing ultrasonic dispersion for 40 min. 2g of ammonia and 1ml of 0.1mol/L Ni (NO) are subsequently added3)2And 2ml of 0.1mol/L Co (NO)3)2Magnetically stirring the solution for 5min, sealing the bottle mouth, and carrying out hydrothermal reaction at 105 ℃ for 12 minh. Then naturally cooling, filtering and washing the obtained product, and drying for 12h at the temperature of 60 ℃.
(3) Taking 10mg of the powder prepared in the last step, adding 10ml of ethanol and 30ml of deionized water, adding a certain amount of 80mg of sodium sulfide, carrying out ultrasonic treatment for 40min, transferring the mixture into a 50ml hydrothermal kettle, and carrying out hydrothermal reaction for 12h at 160 ℃. And then centrifuging and washing the obtained product, and freeze-drying to obtain the product.
Example 3
(1) Dissolving 0.16g of octadecyl trimethyl ammonium bromide in a mixed solution of 30ml of deionized water and 120ml of ethanol, adding 1.5ml of ammonia water and 0.1g of hydroxylated carbon nanotube powder, uniformly mixing in a beaker, and performing ultrasonic dispersion for 40 min. Then 1ml of Tetraethoxysilane (TEOS) is dripped in, and the mixture is stirred for 6 hours by magnetic force with the rotating speed of 60 r/min. Then the product is filtered and washed, and dried for 12h at 60 ℃.
(2) And (3) adding 30mg of the powder material prepared in the previous step into a blue-covered glass bottle, adding 40ml of deionized water, and performing ultrasonic dispersion for 40 min. 1g of urea and 1ml of 0.1mol/L Ni (NO) are subsequently added3)2And 2ml of 0.1mol/L Co (NO)3)2Magnetically stirring the solution for 5min, sealing the bottle mouth, and carrying out hydrothermal reaction at 105 ℃ for 12 h. Then naturally cooling, filtering and washing the obtained product, and drying for 12h at the temperature of 60 ℃.
(3) Taking 10mg of the powder prepared in the last step, adding 10ml of ethanol and 30ml of deionized water, adding a certain amount of 60mg of sodium sulfide, carrying out ultrasonic treatment for 40min, transferring the mixture into a 50ml hydrothermal kettle, and carrying out hydrothermal reaction for 12h at 160 ℃. And then centrifuging and washing the obtained product, and freeze-drying to obtain the product.
The carbon nano tube-cobaltosic sulfide composite material can be prepared by adjusting the process parameters according to the content of the invention, and the performance of the carbon nano tube-cobaltosic sulfide composite material is tested to find that
The sample is detected by a time potential method with different charge and discharge rates, the discharge time of the sample is 300-350s at the charge and discharge rate of 1A/g, and the corresponding capacitance value is 650-700F/g and the capacitance value at 5A/g is 550-600F/g, which remains 80-85%.
The cyclic voltammetry cyclic life test is carried out on the sample for 1600 circles, the material performance is continuously reduced according to a certain rate, and finally 75-85% of the initial capacity is reserved, so that the cyclic stability is good.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A preparation method of a carbon nano tube-cobaltosic sulfide composite material is characterized by comprising the following steps:
step 1, adding deionized water into a carbon nano tube-silicon oxide composite material, performing ultrasonic dispersion, and then adding an alkaline environment promoter and Ni (NO)3)2And Co (NO)3)2Stirring uniformly, carrying out hydrothermal reaction for 10-15h at 90-120 ℃, naturally cooling, carrying out suction filtration, cleaning the obtained product, and drying for 10-15h at 40-80 ℃ to obtain the carbon nano tube-cobalt nickel silicate composite material;
step 2, adding the carbon nano tube-cobalt nickel silicate composite material prepared in the step 1 into a mixed solvent of ethanol and deionized water, and then adding sodium sulfide, wherein the mass ratio of the sodium sulfide to the carbon nano tube-cobalt nickel silicate composite material is (4-8): 1, after uniform dispersion, carrying out hydrothermal reaction for 10-15h at the temperature of 100-200 ℃, and finally centrifuging and cleaning the obtained product, and freeze-drying to obtain the carbon nano tube-cobaltosic sulfide composite material;
the preparation method of the carbon nanotube-silicon oxide composite material in the step 1 comprises the following steps: dissolving a surfactant in a mixed solution of deionized water and ethanol, wherein the concentration of the surfactant is 1-2 gL-1Wherein the volume ratio of the deionized water to the ethanol is 1: (3-5), then adding ammonia water and hydroxylated carbon nanotube powder, wherein: the adding amount of ammonia water is 0.5-2% of the volume of the mixed solution, and the concentration of the carbon nano tube in the mixed solution is 0.5-0.8 g L-1After the dispersion is uniform, dropwise adding tetraethoxysilane, wherein the adding amount of tetraethoxysilane is 0.5-2% of the volume of the mixed solution, stirring and reacting for 5-10 h, and then, filtering, cleaning and washing the productAnd drying for 10-15h at the temperature of 40-80 ℃ to obtain the carbon nano tube-silicon oxide composite material.
2. The method for preparing the carbon nanotube-cobaltosic sulfide composite material according to claim 1, wherein the mass ratio of the alkaline environment promoter to the carbon nanotube-silicon oxide composite material in the step 1 is (1-2): (0.02-0.04), the Ni (NO)3)2The mass ratio of the carbon nano tube to the silicon oxide composite material is 1: (1.6-2.0), Co (NO)3)2The mass ratio of the carbon nano tube to the silicon oxide composite material is 1: (0.8-1.0).
3. The method of claim 1, wherein the surfactant is cetyltrimethylammonium bromide, octadecyltrimethylammonium bromide, or octadecyltrimethylammonium chloride.
4. The method of claim 1, wherein the alkaline environment promoter in step 1 is urea or ammonia.
5. A carbon nano tube-cobaltosic sulfide nickel composite material is characterized by comprising a carbon nano tube and cluster-shaped or nano crystalline cobaltosic sulfide nickel coated on the surface of the carbon nano tube to form a coaxial cable structure, and the coaxial cable structure is prepared according to the following method:
step 1, adding deionized water into a carbon nano tube-silicon oxide composite material, performing ultrasonic dispersion, and then adding an alkaline environment promoter and Ni (NO)3)2And Co (NO)3)2Stirring uniformly, carrying out hydrothermal reaction for 10-15h at 90-120 ℃, naturally cooling, carrying out suction filtration, cleaning the obtained product, and drying for 10-15h at 40-80 ℃ to obtain the carbon nano tube-cobalt nickel silicate composite material;
step 2, adding the carbon nano tube-cobalt nickel silicate composite material prepared in the step 1 into a mixed solvent of ethanol and deionized water, and then adding sodium sulfide, wherein the mass ratio of the sodium sulfide to the carbon nano tube-cobalt nickel silicate composite material is (4-8): 1, after uniform dispersion, carrying out hydrothermal reaction for 10-15h at the temperature of 100-200 ℃, and finally centrifuging and cleaning the obtained product, and freeze-drying to obtain the carbon nano tube-cobaltosic sulfide composite material;
the preparation method of the carbon nanotube-silicon oxide composite material in the step 1 comprises the following steps: dissolving a surfactant in a mixed solution of deionized water and ethanol, wherein the concentration of the surfactant is 1-2 gL-1Wherein the volume ratio of the deionized water to the ethanol is 1: (3-5), then adding ammonia water and hydroxylated carbon nanotube powder, wherein: the adding amount of ammonia water is 0.5-2% of the volume of the mixed solution, and the concentration of the carbon nano tube in the mixed solution is 0.5-0.8 g L-1And after uniform dispersion, dropwise adding tetraethoxysilane, wherein the adding amount of tetraethoxysilane is 0.5-2% of the volume of the mixed solution, stirring and reacting for 5-10 h, then carrying out suction filtration and cleaning on the product, and drying for 10-15h at the temperature of 40-80 ℃ to obtain the carbon nano tube-silicon oxide composite material.
6. The carbon nanotube-cobaltosic sulfide composite material of claim 5, wherein the carbon nanotube-cobaltosic sulfide composite material has a specific capacity of 400-700F/g at a current density of 1A/g.
7. The use of the carbon nanotube-dicobalt sulfide composite material of claim 5 as an electrode material for a supercapacitor.
8. The application of the carbon nanotube-cobaltosic sulfide composite material in the electrode material of the supercapacitor, according to claim 7, wherein the carbon nanotube-cobaltosic sulfide composite material comprises: mixing the carbon nano tube-cobaltosic sulfide nickel composite material with carbon black and polytetrafluoroethylene according to the mass ratio of (5-10) to (1-2), and rolling or coating the mixture to prepare the supercapacitor material.
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