CN110797211B - Carbon cloth loaded CoTe/CoO/Co nanosheet array electrode material and application thereof - Google Patents
Carbon cloth loaded CoTe/CoO/Co nanosheet array electrode material and application thereof Download PDFInfo
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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
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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
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- 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
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Abstract
The invention discloses a carbon cloth loaded CoTe/CoO/Co nanosheet array electrode material and application thereof, and the carbon cloth loaded CoTe/CoO/Co nanosheet array electrode material is prepared by the following method: 1. cleaning the carbon cloth, and preparing a cobalt salt solution; 2. carbon cloth is used as an electrodeposition substrate and a working electrode, Co salt solution is used as electrolyte, and Co (OH) is added by adopting an electrodeposition method2Depositing on the carbon cloth, taking out the carbon cloth after the electrodeposition is finished, cleaning and drying; 3. mixing Te powder and NaBH4Mixing with deionized water uniformly to obtain black liquid, transferring into a hydrothermal kettle, immersing the carbon cloth in the black liquid, carrying out hydrothermal reaction, cooling to room temperature after the reaction is finished, taking out the carbon cloth, cleaning and drying. The material is made of Co (OH)2The nano-sheet array is a sacrificial template, the preparation is carried out by adopting a hydrothermal method, the reaction temperature is low, the energy consumption is low, the formation of the morphology of the CoTe/CoO/Co array nano-sheet is ensured, and the electrochemical performance of the material is fully exerted, so that the material can be used for preparing a pseudo-capacitor electrode and used for electrochemical energy storage.
Description
Technical Field
The invention belongs to the technical field of electrochemical energy storage device materials, and particularly relates to a carbon cloth loaded CoTe/CoO/Co nanosheet array electrode material and application thereof.
Background
With the increase of energy consumption of people, the development of various energy conversion and energy storage equipment is urgent. The super capacitor is a typical energy storage device, has high energy density, is suitable for modern fast-paced life, and has very high commercial value. Capacitors can be classified into electric double layer capacitors and pseudocapacitors from the energy storage mechanism. The double-layer capacitor stores energy by virtue of charges adsorbed on the surface of an electrode material, has excellent long-cycle stability, but the capacity of the electrode depends on the specific surface area of the material, is smaller, and is difficult to meet the requirements of modern people on energy storage devices. Compared with an electric double layer capacitor, the pseudo capacitor stores energy by means of oxidation-reduction reaction of an electrode material, has higher theoretical specific capacity, and is poor in long-cycle stability. Therefore, how to prepare the pseudocapacitor electrode material with high specific capacity and long cycle stability is always a hot point of research.
The powder sample needs to be prepared into an electrode through complex processes such as a conductive agent, a binder and the like, the binder can increase the contact resistance of the material with an electrolyte and a current collector, the electrochemical performance of the material is reduced, and the powder sample is easy to fall off from the current collector in the charging and discharging process, so that the capacity is quickly attenuated. Compared with a powder sample, the array directly grown on the current collector can exert the maximum utilization rate of the material, reduce the agglomeration of the material, and the sample is not easy to fall off from the current collector in the rapid charge and discharge process. The transition metal oxide has high theoretical specific capacity, but the polarization of the electrode material causes the transition metal oxide to have too fast capacity attenuation in the long-cycle process, and the commercial application is difficult to realize. Compared with transition metal oxides, the transition metal telluride has a more stable structure, higher electron mobility and excellent performance in a long-cycle process. However, most of the existing transition metal telluride preparation methods adopt a high-temperature sintering method, and are not easy to prepare arrays directly growing on the current collector, so that a simple and effective method for preparing transition metal telluride arrays is urgently needed.
Disclosure of Invention
Based on the analysis, the invention provides a carbon cloth loaded CoTe/CoO/Co nanosheet array electrode material and application thereof. The material is made of Co (OH)2The nano-sheet array is a sacrificial template, the preparation is carried out by adopting a hydrothermal method, the reaction temperature is low, the energy consumption is low, the formation of the morphology of the CoTe/CoO/Co array nano-sheet is ensured, and the electrochemical performance of the material is fully exerted, so that the material can be used for preparing a pseudo-capacitor electrode and used for electrochemical energy storage.
The technical scheme adopted for realizing the above purpose of the invention is as follows:
a material of a carbon cloth loaded CoTe/CoO/Co nanosheet array is prepared by the following method:
1. cleaning the carbon cloth, and preparing a cobalt salt solution;
2. carbon cloth is used as an electrodeposition substrate and a working electrode, a cobalt salt solution is used as electrolyte, and Co (OH) is added by adopting an electrodeposition method2The nanosheet array is deposited on the carbon cloth, and after electrodeposition is completed, the carbon cloth is taken out, cleaned and dried;
3. mixing Te powder and NaBH4Mixing with deionized water, Te powder and NaBH4The mass ratio of the carbon cloth to the CoTe/CoO/Co nanosheet array electrode material is 1-2.1:2-4, the black liquid is obtained by uniformly mixing, the black liquid is transferred to a hydrothermal kettle, the hydrothermal kettle is sealed after the carbon cloth is immersed in the black liquid, the hydrothermal kettle is heated for hydrothermal reaction, the carbon cloth is taken out after the hydrothermal reaction is finished and is cleaned and dried, and the CoTe/CoO/Co nanosheet array electrode material loaded on the carbon cloth is obtained.
Further, the cobalt salt is cobalt nitrate, cobalt chloride or cobalt sulfate.
Further, when performing electrodeposition in step 2, Ag/AgCl is used as a reference electrode, Pt wire is used as a counter electrode, the voltage window is-1.2V to-0.8V, and the voltage window is 20mV s-1Is cycled for 30 segments at the scan rate.
Further, the temperature of the hydrothermal reaction is 120-180 ℃, and the reaction time is 6-72 h.
Further, in the step 1, when the carbon cloth is cleaned, the carbon cloth is cleaned by ethanol firstly and then by deionized water.
Further, in the steps 2 and 3, when the carbon cloth is cleaned, the carbon cloth is cleaned by deionized water firstly and then cleaned by ethanol.
An application of carbon cloth loaded CoTe/CoO/Co nanosheet array electrode material in electrochemical energy storage.
Compared with the prior art, the invention has the beneficial effects and advantages that:
1. the preparation method of the electrode material is simple, only two steps of reaction are needed, the reaction temperature is low, the energy consumption is low, the raw material source is wide, the price is low, the preparation cost is low, and the preparation method is suitable for industrial production.
2. The CoTe/CoO/Co nanosheet array provided by the invention directly grows on the carbon cloth substrate, and complex preparation processes such as a conductive agent and a binder are omitted.
3. According to the invention, the CoTe/CoO/Co nanosheet array vertically grows on the carbon cloth substrate, so that the self-aggregation of the CoTe/CoO/Co nanosheets is reduced; in the charging and discharging process, the contact area of the CoTe/CoO/Co nanosheets and the electrolyte is large, and meanwhile, the sufficient contact of the vertically-grown CoTe/CoO/Co nanosheet array and the carbon cloth is also beneficial to the rapid transmission of charges.
4. Electrochemical tests show that the CoTe/CoO/Co nanosheet array material prepared by the method has excellent cycling stability, and after 4000 times of rapid charge and discharge, the specific capacity of the electrode still remains 95.2% of the initial value, which is far higher than that of most reported pseudocapacitance materials, such as: CoS @ NiCo2S4(71.7% of the initial value of capacitance remains after 3000 cycles, j. mater. chem.a,2015,3, 24033); CoO @ Co3O4(58.6% of the initial value of capacitance after 4000 cycles; Chemical Engineering Journal 327(2017) 100-108); CoO/Co9S8(75.8% of the initial value of capacitance was retained after 2000 cycles, j. mater. chem.a,2017,5, 18448); co3O4PANI (90% of the initial value of capacitance is retained after 2000 cycles; Applied Surface Science 441(2018) 194-. Therefore, the carbon cloth loaded CoTe/CoO/Co nanosheet array prepared by the method can be used as a continuous and efficient energy storage material, and has extremely high development and application prospects.
Drawings
FIG. 1 shows examples 1 and 2, Co (OH) deposited on a carbon cloth2Low power SEM image of nanoplate array.
FIG. 2 shows Co (OH) deposited on carbon cloth according to examples 1 and 22High power SEM image of nanosheet array.
FIG. 3 is a low-magnification SEM image of the carbon cloth supported CoTe/CoO/Co nanosheet array electrode material prepared in example 1.
FIG. 4 is a high-magnification SEM image of the carbon cloth supported CoTe/CoO/Co nanosheet array electrode material prepared in example 1.
FIG. 5 is an XRD pattern of the carbon cloth supported CoTe/CoO/Co nanosheet array electrode material prepared in example 1.
FIG. 6 is an XPS spectrum of the O element of the CoTe/CoO/Co nanosheet array electrode material prepared in example 1.
FIG. 7 shows Co (OH) prepared in example 12And (3) an XPS (X-ray diffraction) spectrogram of an O element of the nanosheet array electrode material.
FIG. 8 is a TEM image of the CoTe/CoO/Co nanosheet array electrode material prepared in example 1.
FIG. 9 is an HRTEM image of the CoTe/CoO/Co nanosheet array electrode material prepared in example 1.
FIG. 10 is a distribution diagram of cobalt elements on the surface of the CoTe/CoO/Co nanosheet array electrode material prepared in example 1.
FIG. 11 is a surface oxygen distribution diagram of the CoTe/CoO/Co nanosheet array electrode material prepared in example 1.
FIG. 12 is a distribution diagram of tellurium elements on the surface of the CoTe/CoO/Co nanosheet array electrode material prepared in example 1.
FIG. 13 is a cyclic voltammogram of the CoTe/CoO/Co nanosheet array electrode material prepared in example 1.
FIG. 14 is a constant current charging and discharging curve diagram of the CoTe/CoO/Co nanosheet array electrode material prepared in example 1.
FIG. 15 is a graph of rate performance of the CoTe/CoO/Co nanosheet array electrode material prepared in example 1.
FIG. 16 is a graph of the cycling stability performance of the CoTe/CoO/Co nanosheet array electrode material prepared in example 1.
FIG. 17 is an XRD pattern of the CoTe/CoO/Co nanosheet array electrode material prepared in example 2.
Detailed Description
The technical solution of the present invention will be described in detail with reference to specific examples, but the following examples are not intended to limit the scope of the present invention.
Example 1
1. Cutting the carbon cloth into rectangles with regular sizes, then cleaning the carbon cloth with ethanol for three times, and then cleaning the carbon cloth with deionized water for three times for later use;
2. mixing Co (NO)3)2·6H2Adding O into deionized water to prepare 0.1M Co (NO)3)2·6H2O solution;
3. using cyclic voltammetry to convert Co (OH)2Depositing on carbon cloth, using carbon cloth as electrodeposition substrate and working electrode, Ag/AgCl as working electrode, Pt wire as counter electrode, and Co (NO)3)2The solution is electrolyte, the voltage window is-0.8V to-1.2V and is at 20mV s-1The scanning speed of the carbon cloth is circulated for 30 sections, after the electrodeposition is finished, the carbon cloth is taken out, washed with deionized water for three times, then washed with ethanol for three times, and then dried for standby;
4. 77mg of Te powder was weighed and dispersed in 50mL of deionized water, and 110mg of NaBH was rapidly added under magnetic stirring4Continuously stirring the powder for 2min to obtain black liquid;
5. transferring the black liquid into a polytetrafluoroethylene inner container, immersing the carbon cloth obtained in the step 3 into the black liquid, sealing the polytetrafluoroethylene inner container in a reaction kettle, then placing the reaction kettle in an electric heating forced air drying box, starting the electric heating forced air drying box to heat the reaction kettle, keeping the temperature of the black liquid at 160 ℃ for hydrothermal reaction for 12 hours when the temperature of the black liquid in the reaction kettle reaches 160 wind, and taking out the reaction kettle to naturally cool to room temperature after the reaction is finished;
6. and opening the reaction kettle, taking out the carbon cloth, cleaning the carbon cloth with deionized water for three times, cleaning the carbon cloth with ethanol for three times, and drying the carbon cloth to obtain the CoTe/CoO/Co nanosheet array electrode material.
Step 3 of this example was performed to deposit Co (OH)2The carbon cloth of (2) was scanned by a scanning electron microscope, and when the scanning electron microscope was magnified 5000 times, the obtained scanning electron microscope was as shown in FIG. 1, and when the magnification was 60000 times, the obtained scanning electron microscope was as shown in FIG. 2, as can be seen from FIGS. 1 and 2, Co (OH)2Presents a nano-sheet structure and grows uniformly and vertically on the carbon cloth substrate.
The CoTe/CoO/Co nanosheet array electrode material prepared in this example was scanned with a scanning electron microscope, and when the magnification was 5000 times, the obtained scanning electron microscope image was as shown in fig. 3, and when the magnification was 60000 times, the obtained scanning electron microscope image was as shown in fig. 4, as can be seen from fig. 3 and 4, the CoTe/CoO/Co nanosheet array uniformly and vertically grown on the carbon cloth, and Co (oh) remained2Microscopic morphology of nanosheetsThe nano-sheet is presented, the distance between the sheets is reasonable, and more holes are provided, so that the structure of the electrode material and the permeation of electrolyte are maintained, and the capacitance performance and the cycling stability of the CoTe/CoO/Co nano-sheet array electrode material are ensured.
XRD analysis is carried out on the electrode material of the CoTe/CoO/Co nanosheet array prepared in the embodiment, the obtained XRD is shown in figure 5, and as can be seen from figure 5, the electrode material prepared in the embodiment comprises CoTe (JCPDS:34-0420) and Co (JCPDS: 15-0806).
The surface O element of the CoTe/CoO/Co nanosheet array electrode material prepared in this example was subjected to X-ray photoelectron spectroscopy detection, the spectrum of the obtained O element is shown in fig. 6, and after hydrothermal reaction at 160 ℃ for 12 hours, the spectral peak positions of the O element on the nanosheet array surface were 530.18eV and 532.38eV, which correspond to the CoO and the adsorbed water on the material surface, respectively, and Co (oh) was prepared by electrodeposition2The peak position of the O element spectrum of (2) is 531.63eV, as shown in FIG. 7. Apparently, dehydroxylation occurred hydrothermally at 160 ℃, and XPS test showed that hydroxyl oxygen disappeared after hydrothermal treatment, Co (OH)2Having been fully converted to CoO, it can be concluded from the XRD test results that the resulting array after hydrothermal treatment is CoTe/CoO/Co, and CoO is amorphous.
The CoTe/CoO/Co nanosheet array electrode material prepared in this example was scanned with a transmission electron microscope and a high-resolution transmission electron microscope, respectively, and the TEM image obtained is shown in fig. 8, and the HRTEM image obtained is shown in fig. 9. As can be seen from FIG. 8, Co (OH)2After hydrothermal treatment, part of the nanosheet array is converted into an amorphous state, which is supposed to be CoO, and the result is consistent with XPS and XRD test results, and the amorphous CoO has a more stable structure and more active sites and has better performance in the field of energy storage; FIG. 9 shows the interplanar spacings of 0.27nm and 0.19nm, consistent with the interplanar spacings of (002) and (110) of CoTe (JCPDS:34-0420), as measured by 90 ° for the included angle between the (002) and (110) planes, consistent with theoretical values; in addition, FIG. 9 also shows that the 0.17nm interplanar spacing is consistent with the (200) interplanar spacing of zero-valent Co (JCPSD:15-0806), and these results show that we successfully prepared CoTe/CoO/Co composite nano-particles through simple hydrothermal reactionAn array of tiles.
The surface of the CoTe/CoO/Co nanosheet array electrode material prepared in this example was subjected to element distribution detection, and the obtained cobalt element distribution diagram was as shown in fig. 10, the oxygen element distribution diagram was as shown in fig. 11, and the tellurium element distribution diagram was as shown in fig. 12, as can be seen from fig. 10-12, the three elements Co, Te, and O were uniformly distributed on the surface of the electrode material.
The CoTe/CoO/Co nanosheet array electrode material prepared in the embodiment is in the range of 2-20mV s-1The cyclic voltammetry curve obtained is shown in fig. 13, and as can be seen from fig. 13, at different scanning speeds, the CV curve of the CoTe/CoO/Co array has no obvious polarization, which indicates that CoTe/CoO/Co has excellent electron transport property, and the CV curve has obvious redox peaks, which indicates that the electrode material has a typical pseudocapacitance effect.
The CoTe/CoO/Co nanosheet array electrode material prepared in the embodiment is 5-40 mA cm-2The results of constant current charge and discharge tests performed at different current densities are shown in fig. 14. As can be seen from FIG. 14, the constant current charging and discharging curves have better symmetry under different current densities, which indicates that the prepared CoTe/CoO/Co nanosheet array electrode material has a stable reversible process in the charging and discharging processes, and according to 5mA cm-2The area specific capacitance of the electrode material can be up to 1728mF cm by calculating the area specific capacitance C (C ═ Idt/s Δ v, where I is the current, dt is the discharge time, s is the electrode material area, and Δ v is the discharge voltage window) under the current density-2
Specific capacitance tests are carried out on the CoTe/CoO/Co nanosheet array electrode material prepared in the embodiment under different current densities, the voltage window is-0.1-0.5V, and the obtained multiplying power performance graph is shown in FIG. 15. As can be seen from FIG. 15, at 40mAcm-2Under high current, the electrode material still has 706mF cm-2The area specific capacitance is not greatly attenuated along with the increase of the current density, which shows that the prepared CoTe/CoO/Co nanosheet array electrode material has good rate capability.
CoTe/CoO/Co nano prepared in the exampleThe rice chip array electrode material is subjected to a circulating stability test (4000 circles), the voltage window is-0.1-0.5V, and the current density is 40mA cm-2The obtained cycle stability performance is shown in fig. 16, and it can be seen that the capacitance of the electrode retains 95.2% of the initial capacitance after 4000 cycles, thereby showing that the CoTe/CoO/Co nanosheet array electrode material has excellent cycle stability which is far higher than that of many reported pseudocapacitor materials, and has the potential of becoming a commercial material.
Example 2
1. Cutting the carbon cloth into rectangles with regular sizes, then cleaning the carbon cloth with ethanol for three times, and then cleaning the carbon cloth with deionized water for three times for later use;
2. mixing Co (NO)3)2·6H2Adding O into deionized water to prepare 0.1M Co (NO)3)2·6H2O solution;
3. using cyclic voltammetry to convert Co (OH)2Depositing on carbon cloth, using carbon cloth as electrodeposition substrate and working electrode, Ag/AgCl as working electrode, Pt wire as counter electrode, and Co (NO)3)2The solution is electrolyte, the voltage window is-0.8V to-1.2V, 20mV s-1The scanning speed of the carbon cloth is circulated for 30 sections, after the electrolysis is finished, the carbon cloth is taken out and is firstly washed with ethanol for three times, then washed with deionized water for three times, and then dried for standby;
4. 77mg of Te powder was weighed and dispersed in 50mL of deionized water, and 110mg of NaBH was rapidly added under magnetic stirring4Continuously stirring the powder for 2min to obtain black liquid;
5. transferring the black liquid into a polytetrafluoroethylene inner container, immersing the carbon cloth obtained in the step 3 into the black liquid, sealing the polytetrafluoroethylene inner container in a reaction kettle, then placing the reaction kettle in an electric heating forced air drying box, starting the electric heating forced air drying box to heat the reaction kettle, keeping the temperature of the black liquid at 160 ℃ when the temperature of the black liquid in the reaction kettle reaches 160 ℃, carrying out hydrothermal reaction for 72 hours, and taking out the reaction kettle to naturally cool to room temperature after the reaction is finished;
6. and opening the reaction kettle, taking out the carbon cloth, cleaning the carbon cloth with deionized water for three times, cleaning the carbon cloth with ethanol for three times, and drying the carbon cloth to obtain the CoTe/CoO/Co nanosheet array electrode material.
XRD analysis is carried out on the CoTe/CoO/Co nanosheet array electrode material prepared in the example 1, an obtained XRD pattern is shown in FIG. 17, and as can be seen from FIG. 17, when the hydrothermal reaction time is prolonged to 72h, the diffraction peak of zero-valent Co (JCPDS:15-0806) in the CoTe/CoO/Co nanosheet array electrode material is strengthened, so that the content of zero-valent Co in the CoTe/CoO/Co nanosheet array electrode material is increased after the hydrothermal reaction time is prolonged. It can be seen that by controlling the hydrothermal reaction time in step 6, the proportion of the CoTe, CoO and Co can be regulated and controlled, and the optimization of the electrochemical performance of the electrode material is realized.
Claims (7)
1. A carbon cloth loaded CoTe/CoO/Co nanosheet array electrode material is characterized by being prepared by the following method:
1.1, cleaning carbon cloth, and preparing a Co salt solution;
1.2, carbon cloth is used as an electrodeposition substrate and a working electrode, Co salt solution is used as electrolyte, and Co (OH) is prepared by adopting an electrodeposition method2The nanosheet array is deposited on the carbon cloth, and after electrodeposition is completed, the carbon cloth is taken out, cleaned and dried;
1.3, mixing Te powder, NaBH4 and deionized water, wherein the mass ratio of the Te powder to NaBH4 is 1-2.1:2-4, stirring to obtain a black solution, transferring the black solution to a hydrothermal kettle, immersing a carbon cloth in the black solution, sealing the hydrothermal kettle, heating for hydrothermal reaction, cooling to room temperature after the hydrothermal reaction is finished, taking out the carbon cloth, cleaning and drying to obtain the carbon cloth loaded CoTe/CoO/Co nanosheet array electrode material.
2. The carbon cloth-supported CoTe/CoO/Co nanosheet array electrode material of claim 1, wherein: the Co salt is cobalt nitrate, cobalt chloride or cobalt sulfate.
3. The carbon cloth-supported CoTe/CoO/Co nanosheet array electrode material of claim 1, wherein: and (3) when the electrodeposition is carried out in the step 1.2, circulating for 30 sections at a scanning speed of 20mV s-1 by using Ag/AgCl as a reference electrode and Pt wires as a counter electrode and a voltage window of-1.2V to-0.8V.
4. The carbon cloth-supported CoTe/CoO/Co nanosheet array electrode material of claim 1, wherein: the temperature of the hydrothermal reaction is 120-180 ℃, and the reaction time is 6-72 h.
5. The carbon cloth-supported CoTe/CoO/Co nanosheet array electrode material of claim 1, wherein: in the step 1.1, when the carbon cloth is cleaned, the carbon cloth is cleaned by ethanol firstly and then by deionized water.
6. The carbon cloth-supported CoTe/CoO/Co nanosheet array electrode material of claim 1, wherein: in the steps 1.2 and 1.3, when the carbon cloth is cleaned, the carbon cloth is cleaned by deionized water firstly and then cleaned by ethanol.
7. The application of the carbon cloth loaded CoTe/CoO/Co nanosheet array electrode material of claim 1 in electrochemical energy storage.
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