CN110706940B - Three-dimensional porous carbon-manganese oxide core-shell structure material and preparation method and application thereof - Google Patents
Three-dimensional porous carbon-manganese oxide core-shell structure material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a three-dimensional porous carbon-manganese oxide core-shell structure material and a preparation method thereof2Nano structure to prepare C @ MnO of core-shell structure2. The three-dimensional porous carbon-manganese oxide core-shell structure material improves MnO by means of high conductivity and large specific surface of a carbon skeleton2The material has the advantages of high conductivity, large specific capacitance and good cycling stability, and can be used as a supercapacitor electrode material.
Description
Technical Field
The invention belongs to the technical field of energy storage materials, and particularly relates to a three-dimensional porous carbon-manganese oxide core-shell structure material and a preparation method thereof.
Background
The super capacitor is used as a novel electrochemical energy storage device, has high power density, rapid charge and discharge capacity and excellent cycle stability, and has a great application prospect in the fields of flexible wearable electronics, new energy automobiles and the like. Wherein the transition metal oxide is, for example, nanostructured MnO2Due to the characteristics of wide sources, low preparation cost, good stability, high capacity (the theoretical capacity reaches 1370F/g) and the like, the application of the material in the aspect of energy storage is widely concerned by researchers. But with MnO removed2When used as electrode material of super capacitor, MnO2Low electrical conductivity (10)-5-10-6S/cm, Jianan-Gan Wang et al, Progress in Materials Science 74 (2015) 51-124) affects the chemical performance of the supercapacitor, and has the defects of low ion transmission rate, small specific capacitance, poor cycle stability and the like.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a three-dimensional porous carbon-manganese oxide core-shell structure material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a three-dimensional porous carbon-manganese oxide core-shell structure material takes three-dimensional cellular porous carbon prepared by taking cork bark as a raw material as a framework, MnO grows on the surface of the three-dimensional cellular porous carbon2Nano structure to prepare C @ MnO of core-shell structure2(ii) a The specific surface area is 410-780 m2/g。
The preparation method of the three-dimensional porous carbon-manganese oxide core-shell structure material comprises the following steps:
1) preparing a three-dimensional honeycomb porous carbon skeleton: cutting cleaned cork bark into a square body with the length of 10mm, the width of 10mm and the height of 3mm, drying at 60 ℃, soaking in 0.5-1 mol/L potassium hydroxide solution for 3-8 h, taking out, and drying in a vacuum box at 60 ℃ for 24 h; putting the treated cork bark into a ceramic boat with a cover, then placing the ceramic boat into a high-temperature horizontal tube furnace, introducing high-purity Ar gas (the purity reaches 99.999%) according to 300 mL/min when the vacuum degree in the tube furnace reaches 0.1Pa, starting a heating power supply to control the heating rate at 1 ℃/min, heating the furnace to 800-1100 ℃, preserving the temperature for 1-2 h, and then cooling the furnace to room temperature under the protection of the Ar gas to obtain the three-dimensional honeycomb porous carbon skeleton with regular arrangement.
2) Core-shell structure C @ MnO2The preparation of (1): preparing a potassium permanganate solution with the concentration of 0.02-0.06 mol/L, then placing the potassium permanganate solution and the prepared three-dimensional cellular porous carbon skeleton into a polytetrafluoroethylene inner container of a reaction kettle together, then placing the reaction kettle into a drying box, heating to 130-200 ℃, and preserving heat for 2-6 hours, so that MnO is MnO2The nano structure grows on the surface of the carbon skeleton, and is taken out after being cooled along with the furnace to obtain a core-shell structure C @ MnO2Wherein the loading amount of the manganese oxide is 0.0018-0.0024 g.
Table 1 compares the capacitive characteristics of the reported manganese oxide-containing electrode materials
Three-dimensional porous C @ MnO prepared by the invention2The core-shell material has the following advantages:
(1) the invention takes the bark which is low in cost and environment-friendly as the raw material, forms the carbon skeleton array with the honeycomb-shaped porous structure through high-temperature heating decomposition, has dense holes and large specific surface area, and can ensure that the transportation distance of the electrolyte is shorter, the working efficiency of the electrolyte is higher and the mechanical stability is better.
(2) The invention takes three-dimensional porous carbon with excellent conductivity as a conductive framework, and MnO with high specific capacity is grown on the surface of the three-dimensional porous carbon2The MnO can be improved by virtue of high conductivity and large specific surface of the carbon skeleton2The conductivity and electrochemical activity of the whole material fully play the synergistic effect of the core-shell structure.
(3) C @ MnO prepared by the invention2The core-shell structure material has high specific capacity and excellent charge-discharge cycle stability: it is at 1mA/cm2Has a specific capacity of 4.08F/cm at constant current density2(ii) a At 3mA/cm2The specific capacity is 2.98F/cm under the constant current density2(ii) a At 5mA/cm2The specific capacity is 2.92F/cm under the constant current density2. In addition, the material was at 3mA/cm2The specific capacitance has no attenuation after 2000 times of charge and discharge under the constant current density of (2).
Drawings
FIG. 1 is an XRD spectrum of a three-dimensional porous carbon-manganese oxide core-shell structure material synthesized by an example.
FIG. 2 is an EDS map of the three-dimensional porous carbon-manganese oxide core-shell structure material synthesized in the example.
Fig. 3 is an FESEM view (a) and a partial enlarged view (B) of the three-dimensional porous carbon-manganese oxide core-shell structure material synthesized in the example.
FIG. 4 shows three-dimensional porous carbon (C), manganese oxide/nickel foam (MnO)2Nanoneedles) and three-dimensional porous carbon/manganese oxide core-shell structures (C/MnO)2) Cyclic voltammogram of the electrode material.
Fig. 5 is a constant current charge and discharge characteristic diagram of the three-dimensional porous carbon-manganese oxide core-shell structure material.
FIG. 6 is a cycle performance diagram of a three-dimensional porous carbon-manganese oxide core-shell structure material.
Fig. 7 is a constant current charge and discharge characteristic diagram of the three-dimensional porous carbon-manganese oxide core-shell structure material prepared in examples 1 to 3.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Three-dimensional porous carbon/manganese oxide core-shell structure (C/MnO) prepared by adopting three-electrode system pair2) And (5) carrying out an ultra-capacitance test. It is specifically 1M Na2SO4 The solution (room temperature) is used as electrolyte and synthesized C/MnO2The array is used as a working electrode, and a saturated calomel electrode and a platinum sheet electrode are respectively used as a reference electrode and an auxiliary electrode. The cyclic volt-ampere and constant-current charge-discharge test system is an AUTOLAB electrochemical workstation. Wherein the potential range of the charge and discharge test is 0-1.0V, and the current density variation range of the constant current charge and discharge test is 1-5 mA/cm2(ii) a The prepared electrode material is tested by a blue battery test system (LAND-CT2001A) under the condition that the current density is 3mA/cm2The charge-discharge cycle capacity was then carried out 2000 times.
Example 1
Three-dimensional porous carbon-manganese oxide core-shell structure material (C @ MnO)2Nanoneedles) preparation:
1) preparing a three-dimensional honeycomb porous carbon skeleton: cutting cleaned cork bark into square bodies with the length of 10mm, the width of 10mm and the height of 3mm, drying at 60 ℃, soaking in 0.5mol/L potassium hydroxide solution for 6h, taking out, and drying in a vacuum box at 60 ℃ for 24 h; putting the treated cork bark into a ceramic boat with a cover, then putting the ceramic boat into a high-temperature horizontal tube furnace, introducing high-purity Ar gas (the purity reaches 99.999%) at a rate of 300 mL/min when the vacuum degree in the tube furnace reaches 0.1Pa, starting a heating power supply to control the heating rate at 1 ℃/min,heating the furnace to 900 ℃, preserving heat for 1.5 h, and then cooling the furnace to room temperature under the protection of Ar gas to obtain a three-dimensional honeycomb porous carbon skeleton with regular arrangement, wherein the specific surface of the three-dimensional honeycomb porous carbon skeleton is about 1930 m2/g。
2) Core-shell structure C @ MnO2Preparing a nano needle: preparing 40 mL of potassium permanganate solution with the concentration of 0.025mol/L, then placing the potassium permanganate solution and the prepared three-dimensional cellular porous carbon skeleton of about 0.125g into a polytetrafluoroethylene inner container of a reaction kettle together, then placing the reaction kettle into a drying box, heating to 160 ℃, preserving heat for 2 hours, taking out after furnace cooling, and finally drying the sample in vacuum at 60 ℃ for 24 hours to obtain a core-shell structure C @ MnO2And (4) nano needles.
Resulting C @ MnO2The specific surface area of the nanoneedle is 590 m2In terms of a/g, which is at 1mA/cm2Has a specific capacity of 4.08F/cm at constant current density2(ii) a At 3mA/cm2Has a specific capacity of 2.98F/cm at constant current density2(ii) a At 5mA/cm2Has a specific capacity of 2.92F/cm at constant current density2。
FIG. 1 is an XRD spectrum of the synthesized three-dimensional porous carbon-manganese oxide core-shell structure material. As can be seen from the figure, 100 and 031 correspond to manganese oxide peaks, respectively, except for the C peak, indicating that the synthesized sample is a carbon-manganese oxide nanostructure.
FIG. 2 is an EDS map of the synthesized three-dimensional porous carbon-manganese oxide core-shell structure material. As can be seen from the figure, the sample element is composed mainly of C, O, Mn.
Fig. 3 is a FESEM view (a) and a partial enlarged view (B) of the synthesized three-dimensional porous carbon-manganese oxide core-shell structure material. As can be seen in the figure, the nanoneedle-like manganese oxide grows vertically on the carbon nanosheet framework.
FIG. 4 shows three-dimensional porous carbon (C), manganese oxide/nickel foam (MnO)2) And a three-dimensional porous carbon/manganese oxide core-shell structure (C/MnO)2Nanoneedles) electrode material. As can be seen from the figure, under the same sweeping speed (10 mv/s), the capacitance characteristic of the three-dimensional porous carbon/manganese oxide nano core-shell structure material is far superior to that of manganese oxide/nickel foam and a pure three-dimensional porous carbon array.
Fig. 5 is a constant current charge and discharge characteristic diagram of the synthesized three-dimensional porous carbon-manganese oxide core-shell structure material. Equation of the law
The calculation shows that the material is 1mA/cm2Has a specific capacity of 4.08F/cm at constant current density2；3mA/cm2Has a specific capacity of 2.98F/cm at constant current density2；5mA/cm2Has a specific capacity of 2.92F/cm at constant current density2。
FIG. 6 is a cycle performance diagram of the synthesized three-dimensional porous carbon-manganese oxide core-shell structure material. As can be seen, the material is at 3mA/cm2After the charge and discharge for 2000 times under the constant current density, the specific capacitance has no attenuation, and the stability is proved to be good.
Example 2
Three-dimensional porous carbon-manganese oxide core-shell structure material (C @ MnO)2Nanoflower) preparation:
1) preparing a three-dimensional honeycomb porous carbon skeleton: cutting cleaned cork bark into square bodies with the length of 10mm, the width of 10mm and the height of 3mm, drying at 60 ℃, soaking in 0.7 mol/L potassium hydroxide solution for 5 h, taking out, and drying in a vacuum box at 60 ℃ for 24 h; putting the treated cork bark into a ceramic boat with a cover, then placing the ceramic boat into a high-temperature horizontal tube furnace, introducing high-purity Ar gas (the purity reaches 99.999%) according to 300 mL/min when the vacuum degree in the tube furnace reaches 0.1Pa, starting a heating power supply to control the heating rate at 1 ℃/min, heating the furnace to 1000 ℃, preserving the temperature for 1 h, then cooling the furnace to the room temperature under the protection of the Ar gas to obtain a regularly-arranged three-dimensional honeycomb porous carbon skeleton, wherein the specific surface of the three-dimensional honeycomb porous carbon skeleton is about 1780 m2/g。
2) Core-shell structure C @ MnO2Preparing the nanoflower: preparing 40 mL of 0.05mol/L potassium permanganate solution, then placing the potassium permanganate solution and the prepared three-dimensional cellular porous carbon skeleton of about 0.125g into a polytetrafluoroethylene inner container of a reaction kettle together, then placing the reaction kettle into a drying box, heating to 160 ℃, preserving heat for 3 hours, cooling along with a furnace, taking out, and finally vacuum drying the sample at 60 ℃ for 24 hoursObtaining core-shell structure C @ MnO2A nanoflower having a specific surface area of 470 m2/g。
Example 3
Three-dimensional porous carbon-manganese oxide core-shell structure material (C @ MnO)2Nanoparticles) preparation:
1) preparing a three-dimensional honeycomb porous carbon skeleton: cutting cleaned cork bark into square bodies with the length of 10mm, the width of 10mm and the height of 3mm, drying at 60 ℃, soaking in 0.8mol/L potassium hydroxide solution for 4h, taking out, and drying in a vacuum box at 60 ℃ for 24 h; putting the treated cork bark into a ceramic boat with a cover, then placing the ceramic boat into a high-temperature horizontal tube furnace, introducing high-purity Ar gas (the purity reaches 99.999%) according to 300 mL/min when the vacuum degree in the tube furnace reaches 0.1Pa, starting a heating power supply to control the heating rate at 1 ℃/min, heating the furnace to 900 ℃, preserving the heat for 2h, then cooling the furnace to the room temperature under the protection of the Ar gas to obtain a regularly arranged three-dimensional honeycomb porous carbon skeleton, wherein the specific surface of the three-dimensional honeycomb porous carbon skeleton is 2350 m2/g。
2) Core-shell structure C @ MnO2Preparing nano particles: preparing 40 mL of potassium permanganate solution with the concentration of 0.025mol/L, then placing the potassium permanganate solution and the prepared three-dimensional cellular porous carbon skeleton of about 0.125g into a polytetrafluoroethylene inner container of a reaction kettle together, then placing the reaction kettle into a drying box, heating to 130 ℃, preserving heat for 2 hours, taking out after furnace cooling, and finally drying the sample in vacuum at 60 ℃ for 24 hours to obtain a core-shell structure C @ MnO2Nanoparticles having a specific surface area of 710m2/g。
Fig. 7 is a constant current charge/discharge characteristic diagram of the three-dimensional porous carbon-manganese oxide core-shell structure material synthesized in example 1, example 2, and example 3. Equation of the law
The calculation shows that the concentration is 3mA/cm2The specific capacities of the materials obtained in example 1, example 2 and example 3 were 2.98, 1.95 and 2.72F/cm, respectively, at constant current density2。
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (2)
1. A preparation method of a three-dimensional porous carbon-manganese oxide core-shell structure material is characterized by comprising the following steps: adopts three-dimensional honeycomb porous carbon prepared by taking cork bark as a raw material as a framework, and MnO grows on the surface of the three-dimensional honeycomb porous carbon2Nano structure to prepare C @ MnO of core-shell structure2(ii) a Which comprises the following steps:
1) preparing a three-dimensional honeycomb porous carbon skeleton: cutting cleaned cork bark into a square body with the length of 10mm, the width of 10mm and the height of 3mm, drying at 60 ℃, soaking in 0.5-1 mol/L potassium hydroxide solution for 3-8 h, taking out, and drying in a vacuum box at 60 ℃ for 24 h; putting the treated cork bark into a ceramic boat with a cover, then placing the ceramic boat into a high-temperature horizontal tube furnace, introducing high-purity Ar gas at a rate of 300 mL/min when the vacuum degree in the tube furnace reaches 0.1Pa, heating the furnace temperature to 800-1100 ℃ at a rate of 1 ℃/min, preserving the temperature for 1-2 h, and then cooling the cork bark to the room temperature along with the furnace under the protection of the Ar gas to obtain a three-dimensional honeycomb porous carbon skeleton with regular arrangement;
2) core-shell structure C @ MnO2The preparation of (1): preparing a potassium permanganate solution with the concentration of 0.02-0.06 mol/L, then placing the potassium permanganate solution and the prepared three-dimensional cellular porous carbon skeleton into a polytetrafluoroethylene inner container of a reaction kettle together, then placing the reaction kettle into a drying box, heating to 130-200 ℃, preserving heat for 2-6 hours, cooling along with a furnace, and taking out to obtain the core-shell structure C @ MnO2。
2. The preparation method of the three-dimensional porous carbon-manganese oxide core-shell structure material according to claim 1, characterized in that: the specific surface area of the obtained core-shell structure material is 410-780 m2/g。
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