CN113963954B - NHNO nano array, preparation method thereof and application of NHNO nano array in supercapacitor electrode - Google Patents

NHNO nano array, preparation method thereof and application of NHNO nano array in supercapacitor electrode Download PDF

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CN113963954B
CN113963954B CN202111305437.2A CN202111305437A CN113963954B CN 113963954 B CN113963954 B CN 113963954B CN 202111305437 A CN202111305437 A CN 202111305437A CN 113963954 B CN113963954 B CN 113963954B
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nhno
nano
nano array
nanoarray
array
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CN113963954A (en
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朱荣妹
卢加丹
段慧宇
庞欢
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Yangzhou University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

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Abstract

The invention belongs to the field of nano-scale,the NHNO nano array and the preparation method thereof and the application of the NHNO nano array in a super capacitor electrode are disclosed. The invention controls Ni (OH) in the reaction system 2 And HHTP is added to realize the control of the length and the density of the NHNO nano array. The metal organic framework NHNO nano array is obtained through the controllable synthesis method, has good supercapacitor performance, and has important significance in preparing the supercapacitor. Meanwhile, the synthesis method has the characteristics of simple process, low reaction temperature and short time, and is suitable for industrial batch production.

Description

NHNO nano array, preparation method thereof and application of NHNO nano array in supercapacitor electrode
Technical Field
The invention belongs to the field of nano, and relates to an NHNO nano array, a preparation method thereof and application thereof in a super capacitor electrode.
Background
In recent years, the increase in energy demand has been a driving force for the development of energy storage technology due to the growth of population and rapid development of economy. In all energy storage devices, the super capacitor has attracted attention because of its ability to provide higher cycle life, power density, faster redox reaction, and has advantages of environmental friendliness, low cost, and the like. During electrode reaction of a supercapacitor, transport and storage of electrons occur in an electrolyte at or near the surface of an electrode material, and therefore, the microstructure of the electrode material is a key factor affecting the performance of the device. The Metal Organic Framework (MOF) material has the characteristics of simple synthesis method, high porosity, large specific surface area, regular and ordered internal structure and the like, and has a great application prospect in the field of electrochemical energy storage.
Literature research shows that nickel hydroxide is a transition metal hydroxide which is researched more, and when the nickel hydroxide is used as an active substance of a capacitor, the characteristics of good reversibility and high reaction speed in the oxidation and reduction processes of the nickel hydroxide are utilized. In the past, there have been many references to Ni (OH) 2 The research on doping modification is carried out, for example, the research on doping metal elements and rare earth elements, the compound doping of metal elements and the compound doping of rare earth elements and metal elements is carried out. But in Ni (OH) 2 Few reports have been made on the in situ growth of Metal Organic Frameworks (MOFs) on surfaces to synthesize nanoarrays. Therefore, research and developmentAn efficient Ni-based nano array synthesis method with a special structure is very necessary, and particularly, the method has important significance and great challenges when being used for super capacitor electrode materials.
Disclosure of Invention
The invention aims to disclose an NHNO nano-array, a preparation method thereof and application thereof in a super capacitor electrode.
The term "metal-organic framework structure" in the claims and description of the present invention means that the metal-organic framework material is self-assembled from metal ions or metal clusters and organic linking ligands by coordination bonds.
The term "super capacitor" refers to a new type of energy storage device between a conventional capacitor and a rechargeable battery, which has both the fast charging and discharging characteristics of the capacitor and the energy storage characteristics of the battery.
The term "pseudocapacitance" refers to the phenomenon that an electroactive substance undergoes underpotential deposition on a two-dimensional or quasi-two-dimensional space on the surface or in a bulk phase of an electrode, and undergoes highly reversible chemisorption, desorption or oxidation, reduction reactions to produce a capacitance related to the charging potential of the electrode.
One objective of the present invention is to disclose a NHNO nano-array, which is achieved by the following technical solutions.
An NHNO nanoarray on Ni (OH) 2 Ni-HHTP grows on the hexagonal piece in situ,
wherein the Ni-HHTP has a metal-organic framework structure.
Further, the Ni (OH) 2 The thickness of the hexagonal plate is 40 +/-3 nm, the hexagonal plate belongs to the nanometer level, and the large specific surface area is beneficial to ion transmission. ,
further, the length of the NHNO nano array is 74-115nm.
The invention also aims to disclose a preparation method of the NHNO nano-array, which comprises the following steps:
s1, using Ni (OH) 2 Hexagonal plate and Ni (CH) 3 COO) 2 Taking the aqueous solution as a raw material, and carrying out ultrasonic reaction to obtain an intermediate product 1;
s2. Addition of HHTP to H 2 In O, carrying out ultrasonic reaction to obtain an intermediate product 2;
and S3, blending the intermediate product 1 and the intermediate product 2, and heating to react to obtain the NHNO nano-array.
Further, ni (CH) 3 COO) 2 And Ni (OH) 2 The mass ratio of the addition amount of (A) is 1.
Further, ni (OH) 2 The mass ratio to the addition amount of HHTP is 1 to 4, because if Ni (OH) 2 Too much, HHTP will not grow in situ on Ni (OH) 2 Of (2) is provided.
Further, in step S3, the heating reaction temperature is 2-4 o The temperature was gradually increased at a rate of C/min. The heating reaction has a slow heating rate, which is beneficial to more complete reaction. If the temperature rise rate is too fast, the structure of HHTP may be destroyed.
Further, in the step S3, the heating reaction time is 10-15 h.
Furthermore, the ultrasonic reaction time is 5-35 min, which is beneficial to Ni (OH) 2 Sufficient contact with HHTP. The invention also aims to disclose the application of the NHNO nano-array in a supercapacitor electrode.
The invention has the following beneficial effects:
1. the NHNO nano array prepared by the invention has excellent super capacitor performance, can be charged and discharged quickly, namely, stores electric energy efficiently, and has important guiding significance for the technical development of renewable energy sources.
2. The NHNO nanoarrays involved in the present invention can be synthesized at a lower temperature, and can utilize the change of Ni (OH) 2 And HHTP addition amount, so that the morphology of the NHNO nano array is conveniently controlled; in addition, the method has the advantages of simple process, short time and suitability for batch production.
Drawings
FIG. 1 shows TEM images of various materials;
wherein,
FIG. 1 (a) shows Ni (OH) 2 Hexagonal watchA face diagram;
FIG. 1 (b) is a surface map of NHNO nanoarrays prepared in example 1;
FIG. 1 (c) is a surface map of NHNO nanoarrays prepared in example 2;
fig. 1 (d) is a surface map of NHNO nanoarrays prepared in example 3.
Fig. 2 shows a performance test chart of the NHNO nanoarray supercapacitor prepared in example 1;
wherein,
fig. 2 (a) shows a linear sweep voltammetry (CV) curve of NHNO nanoarrays;
fig. 2 (b) shows a cross-current charge-discharge (GCD) curve of the NHNO nanoarray.
Fig. 3 shows a performance test graph of the NHNO nanoarray supercapacitor prepared in example 2;
wherein,
fig. 3 (a) shows a linear sweep voltammetry (CV) curve of NHNO nanoarrays;
fig. 3 (b) shows a cross-current charge-discharge (GCD) curve of the NHNO nanoarray.
Fig. 4 shows a performance test chart of the NHNO nanoarray supercapacitor prepared in example 3;
wherein,
fig. 4 (a) shows a linear sweep voltammetry (CV) curve of NHNO nanoarrays;
fig. 4 (b) shows a cross-current charge-discharge (GCD) curve of the NHNO nano-array.
Detailed Description
In order to more clearly illustrate the technical solution of the present invention, the following examples are given, but the present invention is not limited thereto.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
Example 1
An NHNO nano-array is prepared by in-situ growing Ni-HHTP on Ni (OH) 2 hexagonal plate,
wherein the Ni-HHTP is a metal organic framework structure.
The preparation method of the NHNO nano array comprises the following steps:
s1, weighing 5 mg of Ni (OH) at room temperature 2 2 mL of Ni (CH) was poured into the hexagonal pellets 3 COO) 2 Performing ultrasonic treatment on the aqueous solution (5 mg/mL) for 30 min to obtain an intermediate product 1;
s2, weighing 5 mg of HHTP, pouring the HHTP into 2 mL of deionized water, and carrying out ultrasonic treatment for 5 min to obtain an intermediate product 2;
s3, pouring the intermediate products obtained in the S1 and the S2 into a 10 mL reagent glass bottle. Placing into a muffle furnace, gradually raising the temperature at the speed of 2 ℃/min, and reacting for 12 h at the temperature of 85 ℃. And cooling to room temperature after the reaction is finished, adding sufficient deionized water and acetone for dispersion, and centrifugally separating solids. After washing the solid, the solid turned a blue-black color, and the solid was dried at room temperature overnight for analytical characterization.
FIG. 1 (a) shows Ni (OH) used in the present invention 2 The Transmission Electron Microscope (TEM) examination of the hexagonal plates showed a thickness of 40 nm.
Fig. 1 (b) shows a Transmission Electron Microscopy (TEM) examination of the product of example 1, showing that the prepared NHNO nanoarrays are denser, with the array being about 115nm longer.
Example 2
The NHNO nano array is characterized in that the NHNO nano array is formed by in-situ growth of Ni-HHTP on a Ni (OH) 2 hexagonal sheet,
wherein the Ni-HHTP is a metal organic framework structure.
The preparation method of the NHNO nano array comprises the following steps:
s1, weighing 5 mg of Ni (OH) at room temperature 2 2 mL of Ni (CH) was poured into the hexagonal piece 3 COO) 2 Performing ultrasonic treatment on the aqueous solution (5 mg/mL) for 30 min to obtain an intermediate product 1;
s2, weighing 2.5 mg of HHTP, pouring the HHTP into 2 mL of deionized water, and carrying out ultrasonic treatment for 5 min to obtain an intermediate product 2;
and S3, pouring the intermediate products obtained in the S1 and the S2 into a 10 mL reagent glass bottle. Placing into a muffle furnace, gradually raising the temperature at the speed of 2 ℃/min, and reacting for 12 h at the temperature of 85 ℃. And cooling to room temperature after the reaction is finished, adding sufficient deionized water and acetone for dispersion, and centrifugally separating solids. After washing the solid, the solid turned a blue-black color, and the solid was dried at room temperature overnight for analytical characterization.
Fig. 1 (c) shows a Transmission Electron Microscopy (TEM) examination of the product of example 2, showing that the prepared NHNO nanoarrays are sparse and the arrays are short, about 85 nm.
Example 3
The NHNO nano array is characterized in that the NHNO nano array is formed by in-situ growth of Ni-HHTP on a Ni (OH) 2 hexagonal sheet,
wherein the Ni-HHTP is a metal organic framework structure.
The preparation method of the NHNO nano array comprises the following steps:
s1, weighing 10 mg of Ni (OH) at room temperature 2 2 mL of Ni (CH) was poured into the hexagonal piece 3 COO) 2 Performing ultrasonic treatment on the aqueous solution (5 mg/mL) for 30 min to obtain an intermediate product 1;
s2, weighing 2.5 mg of HHTP, pouring the HHTP into 2 mL of deionized water, and carrying out ultrasonic treatment for 5 min to obtain an intermediate product 2;
s3, pouring the intermediate products obtained in the S1 and the S2 into a 10 mL reagent glass bottle. Placing into a muffle furnace, gradually raising the temperature at the speed of 2 ℃/min, and reacting for 12 h at the temperature of 85 ℃. And cooling to room temperature after the reaction is finished, adding sufficient deionized water and acetone for dispersion, and centrifugally separating solids. After washing the solid, the solid turned a blue-black color, and the solid was dried at room temperature overnight for analytical characterization.
Fig. 1 (d) shows a Transmission Electron Microscope (TEM) image of the product of example 3, showing that the NHNO nanoarrays prepared are sparse and the arrays are short, about 74 nm.
Test example 1
The electrochemical properties of the sample in example 1 used in the supercapacitor electrode were tested in a three-electrode system by cyclic voltammetry and constant current charge-discharge methods, and the specific process was as follows:
electrochemical experiments were performed in model CHI760e electrochemical operationThe test was performed on site using a standard three-electrode test system, with the corresponding working electrode being the sample modified nickel foam electrode obtained herein. The counter electrode was a platinum wire and the reference electrode was mercury/mercury oxide (Hg/HgO). All potentials herein are relative to mercury/mercuric oxide. The electrolyte is 3M KOH solution. All electrochemical tests were at 23 o And (C) performing. At each experiment, all electrodes were tested in 3M KOH solution.
The preparation method of the sample modified foam nickel comprises the following steps:
cutting foamed nickel into size of 1 cm × 5 cm, ultrasonic cleaning with deionized water for 30 min, ultrasonic cleaning with ethanol for 30 min o And C, drying for 3 hours for later use.
8 mg of the NHNO nanoarray prepared in example 1, 0.15 mg of acetylene black were taken and ground in a mortar for 15 min. Adding appropriate amount of isopropanol, and grinding for 15 min. Adding 1-2 drops of Polytetrafluoroethylene (PTFE) emulsion, stirring and then dropping on the surface of the foam nickel to be used. At room temperature overnight, wait for electrochemical testing.
And (3) carrying out cyclic voltammetry and constant current charge and discharge tests on the modified sample foamed nickel in the three-electrode system.
Fig. 2 is a performance test graph of the NHNO nanoarray supercapacitor prepared in example 1. Wherein, fig. 2 (a) shows that the material has an oxidation-reduction peak at 0.4V, which shows that the material has the activity of a pseudo capacitor. Calculated by FIG. 2 (b), the specific capacitances of the NHNO nanoarrays were 127F/g, 110F/g, 90F/g, 76F/g, and 80F/g at current densities of 1A/g, 2A/g, 3A/g, 4A/g, and 5A/g, respectively. The test result shows that the NHNO nano array shows better performance of the super capacitor.
Test example 2
Compared with test example 1, the present test example is different only in that: the NHNO nanoarray prepared in example 1 was replaced with 8 mg of the NHNO nanoarray prepared in example 2.
Fig. 3 is a performance test chart of the NHNO nanoarray supercapacitor prepared in example 2. Wherein, fig. 3 (a) shows that the material has an oxidation-reduction peak at 0.4V, which shows that the material has the activity of a pseudo capacitor. Calculated by FIG. 3 (b), the specific capacitance of the NHNO nanoarray was 289F/g, 248F/g, 222F/g, 198F/g, 180F/g and 175F/g at current densities of 0.5A/g, 1A/g, 2A/g, 3A/g, 4A/g and 5A/g, respectively. The test result shows that the NHNO nano array shows better performance of the super capacitor.
Test example 3
Compared with test example 1, the present test example differs only in that: the NHNO nanoarray prepared in example 1 was replaced with 8 mg of the NHNO nanoarray prepared in example 3.
Fig. 4 is a performance test chart of the NHNO nanoarray supercapacitor prepared in example 3. Wherein, fig. 4 (a) shows that the material has an oxidation-reduction peak at 0.4V, which indicates that the material has the activity of a pseudocapacitor. Calculated by FIG. 4 (b), the specific capacitances of the NHNO nanoarrays were 105F/g, 97F/g, 86F/g, 78F/g, 68F/g and 70F/g at current densities of 0.5A/g, 1A/g, 2A/g, 3A/g, 4A/g and 5A/g, respectively. The test result shows that the NHNO nano array shows better performance of the super capacitor.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (9)

1. The NHNO nano array is characterized in that the NHNO nano array is formed by in-situ growth of Ni-HHTP on a Ni (OH) 2 hexagonal sheet, wherein the Ni-HHTP is a metal-organic framework structure;
the preparation method of the NHNO nano array comprises the following steps:
s1, taking a Ni (OH) 2 hexagonal piece and a Ni (CH 3 COO) 2 aqueous solution as raw materials, and carrying out ultrasonic reaction to obtain an intermediate product 1;
s2, adding HHTP into H2O, and carrying out ultrasonic reaction to obtain an intermediate product 2;
and S3, blending the intermediate product 1 and the intermediate product 2, heating for reaction, washing and settling to obtain the NHNO nano array.
2. The NHNO nanoarray of claim 1, wherein the Ni (OH) 2 hexagonal plate has a thickness of 40 ± 3nm.
3. The NHNO nanoarray of claim 1, wherein the NHNO nanoarray has a length of 74-115nm.
4. The NHNO nanoarray of claim 1, wherein the mass ratio of the addition amount of Ni (OH) 2Ni (CH 3 COO) 2 is 1.
5. The NHNO nanoarray of claim 1, wherein the mass ratio of the addition of Ni (OH) 2 to HHTP is 1.
6. The NHNO nano-array of claim 1, wherein in the step S3, the temperature is gradually increased at a rate of 2-4C/min in the heating reaction.
7. The NHNO nano-array of claim 1, wherein the heating reaction time in step S3 is 10-15 h.
8. The NHNO nanoarray of claim 4, wherein the sonication reaction time is 5-35 min.
9. Use of the NHNO nanoarray of any one of claims 1 to 8 in a supercapacitor electrode.
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