CN110563051A - Preparation method and application of NiCoAl-LDH/N-GO composite material - Google Patents
Preparation method and application of NiCoAl-LDH/N-GO composite material Download PDFInfo
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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 belongs to the technical field of composite material synthesis, relates to preparation of a NiCoAl-LDH composite material, and particularly relates to a preparation method of a NiCoAl-LDH/N-GO composite material, which comprises the following steps: dissolving graphene oxide in deionized water to prepare a solution, ultrasonically dispersing, adding ammonia water, and uniformly stirring; transferring the mixture into a reaction container, reacting for 24-48 h at 120-160 ℃, naturally cooling to room temperature, performing centrifugal separation, sequentially washing solids with water and ethanol, and performing vacuum drying for 24h at 60 ℃ to obtain N-GO; dissolving a nickel source, a cobalt source, an aluminum source and urea in deionized water, adding N-GO in equal proportion, stirring to uniformly disperse the mixture, transferring the mixture into a reaction kettle to react for 24-48 h at 100-120 ℃, naturally cooling to room temperature, and vacuum drying for 24h at 60 ℃ to obtain the catalyst. The invention has simple process and low raw material price, and the prepared material has a regular ultrathin hexagonal lamellar structure, is suitable for being used as an electrode material of a super capacitor, and is easy for industrial production.
Description
Technical Field
The invention belongs to the technical field of composite material synthesis, relates to preparation of a NiCoAl-LDH composite material, and particularly relates to a preparation method and application of a NiCoAl-LDH/N-GO composite material.
Background
In recent years, due to rapid development of electronic products, emerging energy storage devices such as lithium ion batteries and Super Capacitors (SCs) have attracted much attention. Among various energy storage devices, some research has been focused on supercapacitors due to advantages of long life, excellent specific capacitance, and high power density. Thus, by applying different storage mechanisms or enlarging the potential window, the energy density of the supercapacitor is significantly increased. However, the low energy density of ultracapacitors remains an obstacle, which limits their application in various storage devices.
Supercapacitors can be classified into Electric Double Layer Capacitors (EDLCs) and pseudo-capacitive capacitors based on different storage schemes. For the former, charge is stored by the orientation of electrons and ions or dipoles at the electrode/solution interface; in contrast to the former, the charge in the latter is stored based on chemisorption, desorption, or redox reactions of the electrochemically active material on the surface or two-dimensional space of the bulk phase. Carbon-based materials such as graphene oxide and carbon nanotubes have stable properties and a large specific surface area, and are widely used as electrode materials for electric double layer capacitors, while NiCo2O4and the CoAl layered double hydroxide and other pseudo-capacitance materials have excellent performance in specific capacitance due to the rapid electrochemical redox reaction with electrolyte ions. To date, a significant number of pseudocapacitive materials have been explored in search of high specific capacitance and stable cycle life performance.
Layered Double Hydroxides (LDH) in pseudocapacitive materials are advantageous due to their tunable chemical composition, low cost, environmental friendliness and high potential windowAre widely used as suitable redox materials. Thus, the variable valence anion in the layered double hydroxide provides a significant electrochemically active site to create a high faradaic pseudocapacitance. Therefore, the use of LDH as a suitable electrode material is an ideal method to meet the requirements of practical applications. Among the various double metal hydroxides, NiCoAl-LDH is due to its multiple redox states (Ni)2+ / Ni3+and Co2+ / Co3+) And tunable chemical compositions are of particular interest.
in order to optimize the performance of NiCoAl-LDH electrodes, NiCoAl-LDH with abundant active sites must be controllably synthesized in an effort to maximize redox kinetics. Therefore, controlling the composition of NiCoAl-LDH by adjusting the ratio of metal salts is an effective method for improving electrochemical performance. However, their limited rate capability and poor cycling stability have hindered their further use in supercapacitors. On the other hand, graphene materials have high conductivity and rate capability due to sufficient ion diffusion rate, however, increasing the energy density of graphene materials remains a challenge. Therefore, the recombination of LDH with graphene helps to overcome the drawbacks of both materials. Among various graphene materials, reasonably designing a three-dimensional NiCoAl-LDH/aza-graphene N-GO structure is the most potential solution for promoting electron transfer in an electrochemical reaction process.
Disclosure of Invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to utilize graphene oxide for nitrogen doping to prepare N-GO, and then form a three-dimensional NiCoAl-LDH/N-GO by in situ polymerization, thereby obtaining a nanocomposite that can be used as a supercapacitor electrode.
The technical scheme of the invention is as follows:
A preparation method of a NiCoAl-LDH/N-GO composite material comprises the following steps:
A. Dissolving graphene oxide in deionized water to prepare a solution with the concentration of 1-2 mg/mL, carrying out ultrasonic treatment for 0.5-1 h, adding ammonia water according to the volume ratio of 1:10, and stirring uniformly; transferring the mixture into a reaction container, reacting for 24-48 h at 120-160 ℃, preferably reacting for 48h at 160 ℃, naturally cooling to room temperature after the hydrothermal reaction is finished, performing centrifugal separation, sequentially washing the solid with water and ethanol, and performing vacuum drying at 60 ℃ for 24h to prepare N-GO;
B. Dissolving 1-3 mmol of nickel source, 1-3 mmol of cobalt source, 1mmol of aluminum source and 15 mmol of urea in 40 mL of deionized water, adding 25-75 mg of N-GO in equal proportion, stirring to uniformly disperse the mixture, transferring the mixture into a reaction kettle to react at 100-120 ℃ for 24-48 h, preferably at 120 ℃ for 24h, naturally cooling to room temperature, centrifugally separating, washing with water and ethanol for three times, and vacuum drying at 60 ℃ for 24h to obtain the catalyst.
In the better disclosed example of the invention, graphene oxide is dissolved in deionized water to prepare a solution with the concentration of 1 mg/mL for ultrasonic treatment for 1 h.
In the preferred embodiment of the invention, 1mmol of nickel source, 2 mmol of cobalt source, 1mmol of aluminum source and 15 mmol of urea are dissolved in 40 mL of deionized water in the step B, and 75 mg of N-GO is added in equal proportion and stirred to be uniformly dispersed.
In the preferred embodiment of the present invention, the nickel source in step B is Ni (NO)3)2·6H2o or NiCl2·6H2O, the cobalt source is Co (NO)3) ·6H2O or CoCl2·6H2O, the aluminum source is Al (NO)3)3·9H2o or AlCl3。
The NiCoAl-LDH/N-GO composite material prepared by the method is a regular ultrathin hexagonal lamellar nanosheet, and the average transverse size of the NiCoAl-LDH/N-GO composite material is about 100-500 nm.
The prepared NiCoAl-LDH/N-GO composite material is applied to an electrode material of a super capacitor.
(1) Preparation of composite electrode material
Mixing the composite material, the acetylene black conductive agent and the polytetrafluoroethylene dispersion adhesive in a ratio of 8: 1:1, uniformly mixing, uniformly grinding, coating on the treated foamed nickel (1 cm multiplied by 1 cm), drying in an oven at 60-80 ℃ for 12h, and tabletting by using a 10 MPa tablet press to obtain the electrode material, wherein the mass of the sample is about 3 mg.
(2) Testing performance
An electrochemical workstation model CHI660D was used. The test conditions were: a three-electrode system formed by assembling a Saturated Calomel Electrode (SCE) serving as a reference electrode, a platinum electrode serving as a counter electrode and a composite electrode material serving as a working electrode is tested in 2M KOH electrolyte. The electrochemical test is a cyclic voltammetry test (CV), the potential window of a charge-discharge test (GCD) is 0-0.6V, and the frequency range of an electrochemical alternating current impedance analysis (EIS) test is 0.01 Hz-100 KHz.
the reagents used in the invention are all analytically pure and are all commercially available.
Advantageous effects
According to the invention, N-GO is prepared by reducing and doping graphene oxide, and then NiCoAl-LDH is loaded on the surface of N-GO by using an in-situ polymerization method, so that a NiCoAl-LDH/N-GO composite material which can be used as an SC electrode is obtained, and the prepared material has a regular ultrathin hexagonal lamellar structure. The method has the advantages of simple process and low raw material price, and the obtained material is suitable for being used as an electrode material of a super capacitor and is easy for industrial production.
Drawings
FIG. 1 is a scanning electron microscope image, wherein a-b are scanning electron microscope images of N-GO, and c-f are scanning electron microscope images of NiCoAl-LDH/N-GO.
FIG. 2 XRD pattern of NiCoAl-LDH/N-GO.
Detailed Description
the present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
Unless otherwise defined, terms (including technical and scientific terms) used herein should be construed to have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms used herein should be interpreted as having a meaning that is consistent with their meaning in the context of this specification and the relevant art, and should not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Example 1
A preparation method of a NiCoAl-LDH/N-GO composite material comprises the following steps:
A. Dissolving graphene oxide in deionized water to prepare a solution with the concentration of 1 mg/mL, carrying out ultrasonic treatment for 1 h, adding ammonia water according to the volume ratio of 1:10, and uniformly stirring; transferring the mixture into a reaction container to react for 48 hours at 160 ℃, naturally cooling to room temperature after the hydrothermal reaction is finished, centrifugally separating, sequentially washing the solid with water and ethanol, and vacuum-drying for 24 hours at 60 ℃ to obtain N-GO;
B. According to the method, 1mmol of Ni (NO) is dissolved in 40 mL of deionized water3)2·6H2O, 2 mmol of Co (NO)3) ·6H2O, 1mmol of Al (NO)3)3·9H2Adding 75 mg of N-GO into O and 15 mmol of urea in equal proportion, stirring to uniformly disperse the mixture, transferring the mixture into a reaction kettle to react for 24 hours at 120 ℃, naturally cooling to room temperature, carrying out centrifugal separation, washing with water and ethanol for three times, and carrying out vacuum drying for 24 hours at 60 ℃ to obtain the urea.
The prepared NiCoAl-LDH/N-GO composite material is applied to an electrode material of a super capacitor, and the specific capacitance of the material is 1136 F.g-1And the circulation is not attenuated for 5000 times, and the retention rate is 90.10%.
In FIG. 1, it can be seen from a and b that N-GO is a two-dimensional structure with smooth surface. According to c-f, the nano NiCoAl-LDH is composed of irregular and thin hexagonal sheets, and the average transverse size is about 100-500 nm. Meanwhile, it can be obviously seen that a hexagonal sheet structure is loaded on the surface of the N-GO, and the successful preparation of the binary composite material NiCoAl-LDH/N-GO is proved.
In FIG. 2, (003) is a characteristic peak of NiCoAl-LDH/N-GO.
example 2
a preparation method of a NiCoAl-LDH/N-GO composite material comprises the following steps:
A. Dissolving graphene oxide in deionized water to prepare a solution with the concentration of 2 mg/mL, carrying out ultrasonic treatment for 0.5 h, adding ammonia water according to the volume ratio of 1:10, and uniformly stirring; transferring the mixture into a reaction container to react for 24 hours at 120 ℃, naturally cooling to room temperature after the hydrothermal reaction is finished, centrifugally separating, sequentially washing the solid with water and ethanol, and vacuum-drying for 24 hours at 60 ℃ to obtain N-GO;
B. According to the method, 3 mmol of Ni (NO) is dissolved in 40 mL of deionized water3)2·6H2o, 3 mmol of Co (NO)3) ·6H2O, 1mmol of Al (NO)3)3·9H2Adding 25-75 mg of N-GO into O and 15 mmol of urea in equal proportion, stirring to uniformly disperse the mixture, transferring the mixture into a reaction kettle to react for 48 hours at 100 ℃, naturally cooling to room temperature, performing centrifugal separation, washing with water and ethanol for three times, and performing vacuum drying for 24 hours at 60 ℃ to obtain the urea.
The prepared NiCoAl-LDH/N-GO composite material is applied to an electrode material of a super capacitor, and the specific capacitance of the material is 1037F g-15000 cycles did not decay, with a retention of 84.61%.
example 3
A preparation method of a NiCoAl-LDH/N-GO composite material comprises the following steps:
A. Dissolving graphene oxide in deionized water to prepare a solution with the concentration of 1 mg/mL, carrying out ultrasonic treatment for 0.5 h, adding ammonia water according to the volume ratio of 1:10, and uniformly stirring; transferring the mixture into a reaction container to react for 24 hours at 120 ℃, naturally cooling to room temperature after the hydrothermal reaction is finished, centrifugally separating, sequentially washing the solid with water and ethanol, and vacuum-drying for 24 hours at 60 ℃ to obtain N-GO;
B. according to the method, 1mmol of Ni (NO) is dissolved in 40 mL of deionized water3)2·6H2O, 1mmol of Co (NO)3) ·6H2O, 1mmol of Al (NO)3)3·9H2Adding 25 mg of N-GO into O and 15 mmol of urea in equal proportion, stirring to uniformly disperse the mixture, transferring the mixture into a reaction kettle to react for 24 hours at 100 ℃, naturally cooling to room temperature, carrying out centrifugal separation, washing with water and ethanol for three times, and carrying out vacuum drying for 24 hours at 60 ℃ to obtain the urea.
The prepared NiCoAl-LDH/N-GO composite material is applied to an electrode material of a super capacitor, and the specific capacitance of the composite material is 985 F.g-15000 cycles did not decay, with a retention of 76.47%.
Example 4
A preparation method of a NiCoAl-LDH/N-GO composite material comprises the following steps:
A. Dissolving graphene oxide in deionized water to prepare a solution with the concentration of 2 mg/mL, carrying out ultrasonic treatment for 1 h, adding ammonia water according to the volume ratio of 1:10, and uniformly stirring; transferring the mixture into a reaction container to react for 48 hours at 160 ℃, naturally cooling to room temperature after the hydrothermal reaction is finished, centrifugally separating, sequentially washing the solid with water and ethanol, and vacuum-drying for 24 hours at 60 ℃ to obtain N-GO;
B. According to the method, 3 mmol of NiCl is dissolved in 40 mL of deionized water2·6H2O, 3 mmol of CoCl2·6H2O, 1mmol of AlCl3And 15 mmol of urea, adding 75 mg of N-GO in equal proportion, stirring to uniformly disperse the urea, transferring the mixture into a reaction kettle to react for 48 hours at 120 ℃, naturally cooling to room temperature, carrying out centrifugal separation, washing with water and ethanol for three times, and carrying out vacuum drying for 24 hours at 60 ℃ to obtain the urea.
The prepared NiCoAl-LDH/N-GO composite material is applied to an electrode material of a super capacitor, and the specific capacitance of the composite material is 1086 F.g-1And the circulation does not decay for 5000 times, and the retention rate is 86.73 percent.
Example 5
A preparation method of a NiCoAl-LDH/N-GO composite material comprises the following steps:
A. Dissolving graphene oxide in deionized water to prepare a solution with the concentration of 1 mg/mL, carrying out ultrasonic treatment for 0.5 h, adding ammonia water according to the volume ratio of 1:10, and uniformly stirring; transferring the mixture into a reaction container to react for 24 hours at 120 ℃, naturally cooling to room temperature after the hydrothermal reaction is finished, centrifugally separating, sequentially washing the solid with water and ethanol, and vacuum-drying for 24 hours at 60 ℃ to obtain N-GO;
B. According to the method, 3 mmol of NiCl is dissolved in 40 mL of deionized water2·6H2O, 3 mmol of CoCl2·6H2O, 1mmol of AlCl3And 15 mmol of urea, adding 25-75 mg of N-GO in equal proportion, stirring to uniformly disperse the urea, transferring the mixture into a reaction kettle to react for 24 hours at 100 ℃, naturally cooling to room temperature, performing centrifugal separation, washing with water and ethanol for three times, and performing vacuum drying at 60 ℃ for 24 hours to obtain the urea.
The prepared NiCoAl-LDH/N-GO composite material is applied to an electrode material of a super capacitor,Its specific capacitance is 1021F g-1And the circulation does not decay for 5000 times, and the retention rate is 82.64 percent.
Example 6
A preparation method of a NiCoAl-LDH/N-GO composite material comprises the following steps:
A. Dissolving graphene oxide in deionized water to prepare a solution with the concentration of 2 mg/mL, carrying out ultrasonic treatment for 1 h, adding ammonia water according to the volume ratio of 1:10, and uniformly stirring; transferring the mixture into a reaction container to react for 48 hours at 160 ℃, naturally cooling to room temperature after the hydrothermal reaction is finished, centrifugally separating, sequentially washing the solid with water and ethanol, and vacuum-drying for 24 hours at 60 ℃ to obtain N-GO;
B. According to the method, 1mmol of NiCl is dissolved in 40 mL of deionized water2·6H2o, 1mmol of CoCl2·6H2O, 1mmol of AlCl3and 15 mmol of urea, adding 25-75 mg of N-GO in equal proportion, stirring to uniformly disperse the urea, transferring the mixture into a reaction kettle to react for 24 hours at 100 ℃, naturally cooling to room temperature, performing centrifugal separation, washing with water and ethanol for three times, and performing vacuum drying at 60 ℃ for 24 hours to obtain the urea.
The prepared NiCoAl-LDH/N-GO composite material is applied to an electrode material of a super capacitor, and the specific capacitance of the material is 997 F.g-1And the circulation does not decay for 5000 times, and the retention rate is 80.28 percent.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (8)
1. A preparation method of a NiCoAl-LDH/N-GO composite material is characterized by comprising the following steps:
Dissolving graphene oxide in deionized water to prepare a solution with the concentration of 1-2 mg/mL, carrying out ultrasonic treatment for 0.5-1 h, adding ammonia water according to the volume ratio of 1:10, and stirring uniformly; transferring the mixture into a reaction container, reacting for 24-48 h at 120-160 ℃, naturally cooling to room temperature after the hydrothermal reaction is finished, performing centrifugal separation, sequentially washing solids with water and ethanol, and performing vacuum drying for 24h at 60 ℃ to obtain N-GO;
Dissolving 1-3 mmol of nickel source, 1-3 mmol of cobalt source, 1mmol of aluminum source and 15 mmol of urea in 40 mL of deionized water, adding 25-75 mg of N-GO in equal proportion, stirring to uniformly disperse the mixture, transferring the mixture into a reaction kettle to react for 24-48 h at 100-120 ℃, naturally cooling to room temperature, carrying out centrifugal separation, washing with water and ethanol for three times, and carrying out vacuum drying at 60 ℃ for 24h to obtain the catalyst.
2. The method for preparing NiCoAl-LDH/N-GO composite material according to claim 1, wherein: and step A, dissolving graphene oxide in deionized water to prepare a solution with the concentration of 1 mg/mL, and carrying out ultrasonic treatment for 1 h.
3. The method for preparing NiCoAl-LDH/N-GO composite material according to claim 1, wherein: transferring the mixture into a reaction vessel for reaction for 48 hours at 160 ℃.
4. the method for preparing NiCoAl-LDH/N-GO composite material according to claim 1, wherein: and B, dissolving 1mmol of nickel source, 2 mmol of cobalt source, 1mmol of aluminum source and 15 mmol of urea in 40 mL of deionized water, adding 75 mg of N-GO in equal proportion, and stirring to uniformly disperse the mixture.
5. The method for preparing NiCoAl-LDH/N-GO composite material according to claim 1, wherein: step B the nickel source is Ni (NO)3)2·6H2O or NiCl2·6H2O, the cobalt source is Co (NO)3) ·6H2O or CoCl2·6H2o, the aluminum source is Al (NO)3)3·9H2O or AlCl3。
6. the method for preparing NiCoAl-LDH/N-GO composite material according to claim 1, wherein: transferring the mixture into a reaction kettle for reaction at 120 ℃ for 24 hours.
7. A NiCoAl-LDH/N-GO composite material made by the method of any one of claims 1 to 6.
8. The NiCoAl-LDH/N-GO composite material of claim 7, wherein: the method is applied to an electrode material of a super capacitor.
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