CN109950051B - Spherical core-shell structure C @ MnO2@ NiAl-LDH nano composite and preparation method thereof - Google Patents
Spherical core-shell structure C @ MnO2@ NiAl-LDH nano composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a spherical core-shell structure C @ MnO2The @ NiAl-LDH nano-composite and the preparation method thereof are characterized in that: the nano composite is formed by wrapping MnO on a C nanosphere2In MnO of2The outer is wrapped with NiAl-LDH nano-sheets. C @ MnO of spherical core-shell structure prepared by the invention2The @ NiAl-LDH nano composite has excellent supercapacitor property, and the production process is simple and safe, strong in operability and excellent in repeatability.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to C @ MnO with a spherical core-shell structure2A @ NiAl-LDH nano-composite and a preparation method thereof.
Background
The super capacitor is used as an energy storage device which is green, pollution-free and low in cost, attracts extensive attention and interest of researchers in various countries, and simultaneously puts higher requirements on active electrode materials of the super capacitor. In order to be able to produce a high-performance supercapacitor, phases are requiredThe electrode material has large specific surface area and pore volume, excellent conductivity and good cycling stability. The carbon material is a material with wide application, has the advantages of rich raw materials, high conductivity and the like, and is considered as a good electrode material of the supercapacitor by a plurality of researchers, but the carbon material has a special structure, the rate capability of the carbon material is gradually weakened, and the extensibility of the carbon material is poor, so that the application of the carbon material in the field of the supercapacitor is limited. Some metal oxides, e.g. RuO2Shows excellent electrochemical performance of the super capacitor, but the application of Ru in a plurality of fields is limited by the scarcity of Ru as a noble metal. The transition metal oxide or transition metal hydroxide can replace the noble metal oxide or hydroxide, and has the advantages of low price, no pollution to the environment and higher specific capacitance, such as MnO2、Mn2O3、NiO、Fe3O4Etc. wherein MnO is2Is a transition metal oxide with more development prospect. The Shu subject group utilizes beta-cyclodextrin and divalent manganese salt to prepare C @ MnO with a core-shell structure by a two-step hydrothermal method2A composite material as an electrode active material for a supercapacitor, which has a specific capacitance of 396.4F/g (H Cheng, S X ZHao, F Y Yi, D Shu, C He. journal of Alloys and Compounds,2019,779: 550-. Yu subject group utilizes N-doped hollow carbon spheres as a reducing agent and potassium permanganate as an oxidizing agent to prepare controllable core-shell structure C @ MnO2A composite material, which is used as an electrode active material and has a specific capacitance of 392F/G at 0.5A/G (T Liu, C J Jiang, W You, J G Yu. journal of Materials Chemistry A,2017,5(18): 8635-. CN108039287A discloses Fe with a double-shell structure obtained by a gradual coating method3O4/C/MnO2The specific capacitance of the composite material at 0.5A/g is 340F/g. Above for C @ MnO2The related composite material is lower in specific capacitance when being used as an electrode active material in a super capacitor, so that C @ MnO with more excellent performance is developed2Basic composite materials are highly desirable.
Disclosure of Invention
To g inIn order to overcome the defects of the prior art, the invention aims to provide C @ MnO with a spherical core-shell structure2The @ NiAl-LDH nano composite material and its preparation process aim at obtaining composite material with high specific capacitance performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention discloses a spherical core-shell structure C @ MnO2The @ NiAl-LDH nano composite is formed by wrapping MnO on a C nanosphere2In MnO2The external coating of the NiAl-LDH nano-sheet has a specific surface area of 90-120m2/g。
The invention relates to a spherical core-shell structure C @ MnO2The preparation method of the @ NiAl-LDH nano composite comprises the following steps: firstly, C ball is used as a template agent, a reducing agent and KMnO4Synthesis of C @ MnO as an oxidizing agent2A composite material; then performing a coprecipitation method on the mixture at C @ MnO2Depositing NiAl-LDH nano-sheets on the composite material to obtain the spherical core-shell structure C @ MnO2@ NiAl-LDH nanocomposite. The method specifically comprises the following steps:
(1) preparation of C balls
Ultrasonically dispersing 7.2g of glucose in 80mL of deionized water to form a uniform solution, then transferring the uniform solution to a stainless steel reaction kettle, and carrying out oven reaction at 180 ℃ for 6 hours; after the reaction is finished, naturally cooling to room temperature, washing the obtained product, and carrying out vacuum drying at 80 ℃ to obtain a C ball;
(2) preparation of C @ MnO2Composite material
Ultrasonically dispersing 1.0g C spheres in 70mL deionized water, and adding 0.5g KMnO4And stirring uniformly; transferring the obtained solution into a stainless steel reaction kettle, and carrying out oven reaction at 120 ℃ for 12 hours; after the reaction is finished, naturally cooling to room temperature, washing the obtained product, and drying the product in vacuum at 80 ℃ to obtain C @ MnO2A composite material;
(3) preparation of C @ MnO2@ NiAl-LDH nanocomposite:
completely dissolving 0.131g to 0.524g of nickel nitrate hexahydrate and 0.085g to 0.338g of aluminum nitrate nonahydrate in 25mL of deionized water to form a solution A; 0.1g C @ MnO2Composite material, 0.043g-0.170g Na2CO3And 0.063g to 0.252g NaOH was completely dissolved in 25mL deionized water to form solution B; dropwise adding the solution A into the solution B and continuously stirring; transferring the obtained suspension into a stainless steel reaction kettle, and reacting for 6 hours in an oven at 120 ℃; after the reaction is finished, naturally cooling to room temperature, washing the obtained product, and drying the product in vacuum at 80 ℃ to obtain the spherical core-shell structure C @ MnO2@ NiAl-LDH nanocomposite.
Spherical core-shell structure C @ MnO prepared by the invention2The @ NiAl-LDH nanocomposite can be used as an electrode active material in a supercapacitor.
Compared with the prior art, the invention has the beneficial effects that:
1. the method can obtain the C @ MnO with the spherical core-shell structure by adopting a simple hydrothermal method by only using seven raw materials of glucose, potassium permanganate, sodium carbonate, sodium hydroxide, nickel nitrate hexahydrate, aluminum nitrate nonahydrate and deionized water2The @ NiAl-LDH nano-composite does not use any organic solvent and auxiliary agent in the process, and realizes a clean production process without pollution.
2. C @ MnO of spherical core-shell structure prepared by the invention2The @ NiAl-LDH nano composite has excellent super capacitor property, and under the specific working current of 1.0A/g, the specific capacitance is 990F/g, and the specific surface area is 90-120m2The specific capacitance property is improved by the aid of the specific capacitance per gram, and binding sites of the active material can be increased.
3. The invention is used for preparing spherical core-shell structure C @ MnO2In the process of the @ NiAl-LDH nano compound, glucose is used as a carbon source, other template agents do not need to be introduced, and the production process is simple and safe, strong in operability and excellent in repeatability.
Drawings
FIG. 1 is an XRD pattern of a nanocomposite prepared according to example 1 of the present invention;
FIG. 2 is a TEM image of a nanocomposite prepared in example 1 of the present invention;
FIG. 3 is a graph of Cyclic Voltammetry (CV) of the nanocomposite prepared in examples 1 to 3 of the present invention;
FIG. 4 is a graph of constant current charging and discharging (GCD) of the nanocomposites prepared in examples 1-3 of the present invention.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
For the spherical core-shell structure C @ MnO prepared in the following example2The electrochemical test method of the @ NiAl-LDH nanocomposite electrode material comprises the following steps: cyclic Voltammetry (CV), Galvanostatic Charging and Discharging (GCD).
When the invention is used for testing the performance of the super capacitor, the three electrode systems are as follows: silver/silver chloride (Ag/AgCl) electrode as reference electrode, platinum wire (Pt) electrode as counter electrode, C @ MnO2The electrode prepared by uniformly coating the @ NiAl-LDH nano composite on the foamed nickel is used as a working electrode. The electrolyte solution is 6mol/L KOH solution. The electrochemical test was performed on an electrochemical workstation (CHI-660D, shanghai chenghua).
Example 1
C @ MnO of spherical core-shell structure2The preparation method of the @ NiAl-LDH nano composite comprises the following steps:
(1) preparation of C balls
Ultrasonically dispersing 7.2g of glucose in 80mL of deionized water to form a uniform solution, then transferring the uniform solution to a stainless steel reaction kettle, and carrying out oven reaction at 180 ℃ for 6 hours; after the reaction is finished, naturally cooling to room temperature, alternately washing the obtained product with deionized water and absolute ethyl alcohol for three times respectively, and drying in a vacuum oven at 80 ℃ for 12 hours to obtain a C ball;
(2) preparation of C @ MnO2Composite material
Ultrasonically dispersing 1.0g C spheres in 70mL deionized water, and adding 0.5g KMnO4And stirring uniformly; transferring the obtained solution into a stainless steel reaction kettle, and carrying out oven reaction at 120 ℃ for 12 hours; after the reaction is finished, naturally cooling to room temperature, alternately washing the obtained product with deionized water and absolute ethyl alcohol for three times respectively, and drying in a vacuum oven at 80 ℃ for 12 hours to obtain C @ MnO2A composite material;
(3) preparation of C @ MnO2@ NiAl-LDH nanocomposite:
completely dissolving 0.262g of nickel nitrate hexahydrate and 0.169g of aluminum nitrate nonahydrate in 25mL of deionized water to form solution A; 0.1g C @ MnO2Composite material, 0.085g Na2CO3And 0.126g NaOH was completely dissolved in 25mL deionized water to form solution B; dropwise adding the solution A into the solution B and continuously stirring; transferring the obtained suspension into a stainless steel reaction kettle, and reacting for 6 hours in an oven at 120 ℃; after the reaction is finished, naturally cooling to room temperature, alternately washing the obtained product with deionized water and absolute ethyl alcohol for three times respectively, and drying in a vacuum oven at 80 ℃ for 12 hours to obtain the spherical core-shell structure C @ MnO2@ NiAl-LDH nanocomposite.
Referring to the XRD and TEM images of FIGS. 1 and 2, the C @ MnO of the spherical core-shell structure prepared in this example can be seen2The @ NiAl-LDH nano-composite is presented by wrapping MnO on a C ball2Then MnO was added2The NiAl-LDH nano-sheets are wrapped on the surface of the substrate, and no impurity phase peak is found, which shows that the purity of the product is higher. The product obtained in this example was tested to have a specific surface area of 120m2/g。
Example 2
C @ MnO of spherical core-shell structure2The preparation method of the @ NiAl-LDH nano composite comprises the following steps:
(1) preparation of C balls
Same as in example 1.
(2) Preparation of C @ MnO2Composite material
Same as in example 1.
(3) Preparation of C @ MnO2@ NiAl-LDH nanocomposite
Completely dissolving 0.131g of nickel nitrate hexahydrate and 0.085g of aluminum nitrate nonahydrate in 25mL of deionized water to form a solution A; 0.1g C @ MnO2Composite material, 0.043g Na2CO3And 0.063g NaOH was completely dissolved in 25mL deionized water to form solution B; dropwise adding the solution A into the solution B and continuously stirring; transferring the obtained suspension into a stainless steel reaction kettle, and reacting for 6 hours in an oven at 120 ℃; after the reaction is finished, naturally cooling to room temperature, and obtaining a productWashing deionized water and absolute ethyl alcohol alternately for three times respectively, and drying in a vacuum oven at 80 ℃ for 12 hours to obtain the spherical core-shell structure C @ MnO2@ NiAl-LDH nanocomposite.
The characteristics show that the C @ MnO of the spherical core-shell structure prepared in the embodiment2The @ NiAl-LDH nano-composite is presented by wrapping MnO on a C ball2Then MnO was added2The NiAl-LDH nano-sheets are wrapped on the surface of the substrate, and no impurity phase peak is found, which shows that the purity of the product is higher. The product obtained in this example was tested to have a specific surface area of 95m2/g。
Example 3
C @ MnO of spherical core-shell structure2The preparation method of the @ NiAl-LDH nano composite comprises the following steps:
(1) preparation of C balls
Same as in example 1.
(2) Preparation of C @ MnO2Composite material
Same as in example 1.
(3) Preparation of C @ MnO2@ NiAl-LDH nanocomposite:
completely dissolving 0.524g of nickel nitrate hexahydrate and 0.338g of aluminum nitrate nonahydrate in 25mL of deionized water to form solution A; 0.1g C @ MnO2Composite material, 0.170g Na2CO3And 0.252g NaOH was completely dissolved in 25mL deionized water to form solution B; dropwise adding the solution A into the solution B and continuously stirring; transferring the obtained suspension into a stainless steel reaction kettle, and reacting for 6 hours in an oven at 120 ℃; after the reaction is finished, naturally cooling to room temperature, alternately washing the obtained product with deionized water and absolute ethyl alcohol for three times respectively, and drying in a vacuum oven at 80 ℃ for 12 hours to obtain the spherical core-shell structure C @ MnO2@ NiAl-LDH nanocomposite.
The characteristics show that the C @ MnO of the spherical core-shell structure prepared in the embodiment2The @ NiAl-LDH nano-composite is presented by wrapping MnO on a C ball2Then MnO was added2The NiAl-LDH nano-sheets are wrapped on the surface of the substrate, and no impurity phase peak is found, which shows that the purity of the product is higher. The product obtained in this example was tested to have a specific surface area of 97m2/g。
The capacitive properties of the products obtained in examples 1 to 3 were determined as follows:
(1) c @ MnO of spherical core-shell structure2Weighing 6mg of the @ NiAl-LDH nano-composite powder, acetylene black and polytetrafluoroethylene micro powder in a mass ratio of 8:1:1, putting the weighed materials into a mortar, adding 4 drops of N-methylpyrrolidone, and fully and uniformly grinding the materials;
(2) preparing a standard foam nickel of 1cm multiplied by 3cm, sequentially treating with deionized water and ethanol for three times, drying and weighing;
(3) uniformly coating the sample obtained in the step 1 on foamed nickel, and drying at 60 ℃ for 12 hours;
(4) tabletting the dried foam nickel sample under the pressure of 10MPa, and weighing;
(5) under 6mol/L KOH electrolyte, C @ MnO of spherical core-shell structure is treated by an electrochemical workstation2The capacitive properties of the @ NiAl-LDH nanocomposite were tested with operating currents of 10A, 8A, 5A, 3A, 1A, respectively.
FIGS. 3 and 4 are C @ MnO of spherical core-shell structures prepared in examples 1-32The comparison graph of the Circulating Voltammogram (CV) and the constant current charge-discharge diagram (GCD) of the @ NiAl-LDH nanocomposite material. It can be seen that the specific capacitances C of the samples obtained in examples 1-3 were 990F/g, 547F/g and 523F/g, respectively, at a specific operating current of 1.0A/g. Further, C @ MnO of spherical core-shell structure obtained in example 12The specific capacitance C of the @ NiAl-LDH nano-composite is 597.62F/g, 629.87F/g, 712.11F/g and 855.19F/g respectively under specific working currents of 10A/g, 8A/g, 5A/g and 3A/g.
Claims (1)
1. Spherical core-shell structure C @ MnO2The preparation method of the @ NiAl-LDH nano composite is characterized by comprising the following steps: the nano composite is formed by wrapping MnO on a C nanosphere2In MnO of2The outer package is wrapped with NiAl-LDH nano sheets; the specific surface area of the nano composite is 90-120m2/g;
The preparation method of the nano-composite comprises the following steps: firstly, C ball is used as a template agent, a reducing agent and KMnO4Synthesis of C @ MnO as an oxidizing agent2A composite material; then performing a coprecipitation method on the mixture at C @ MnO2Depositing NiAl-LDH nano-sheets on the composite material to obtain the spherical core-shell structure C @ MnO2@ NiAl-LDH nanocomposite; the method specifically comprises the following steps:
(1) preparation of C balls
Ultrasonically dispersing 7.2g of glucose in 80mL of deionized water to form a uniform solution, then transferring the uniform solution to a stainless steel reaction kettle, and carrying out oven reaction at 180 ℃ for 6 hours; after the reaction is finished, naturally cooling to room temperature, washing the obtained product, and carrying out vacuum drying at 80 ℃ to obtain a C ball;
(2) preparation of C @ MnO2Composite material
Ultrasonically dispersing 1.0g C spheres in 70mL deionized water, and adding 0.5g KMnO4And stirring uniformly; transferring the obtained solution into a stainless steel reaction kettle, and carrying out oven reaction at 120 ℃ for 12 hours; after the reaction is finished, naturally cooling to room temperature, washing the obtained product, and drying the product in vacuum at 80 ℃ to obtain C @ MnO2A composite material;
(3) preparation of C @ MnO2@ NiAl-LDH nanocomposite
Completely dissolving 0.131g to 0.524g of nickel nitrate hexahydrate and 0.085g to 0.338g of aluminum nitrate nonahydrate in 25mL of deionized water to form a solution A; 0.1g C @ MnO2Composite material, 0.043g-0.170g Na2CO3And 0.063g to 0.252g NaOH was completely dissolved in 25mL deionized water to form solution B; dropwise adding the solution A into the solution B and continuously stirring; transferring the obtained suspension into a stainless steel reaction kettle, and reacting for 6 hours in an oven at 120 ℃; after the reaction is finished, naturally cooling to room temperature, washing the obtained product, and drying the product in vacuum at 80 ℃ to obtain the spherical core-shell structure C @ MnO2@ NiAl-LDH nanocomposite.
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