CN113948316B - Preparation method and application of three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon - Google Patents
Preparation method and application of three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon 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 discloses a preparation method and application of three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon, wherein the preparation method comprises the following steps: s1: preparation of nitrogen source and phosphorus source precursors: firstly, reacting melamine with phytic acid according to a certain molar ratio, and obtaining a nitrogen source and a phosphorus source precursor after the reaction is finished; s2: pretreatment of reactants: grinding phenanthrene, melamine, phytic acid polymer, potassium sulfate and potassium oxalate activator according to a certain mass ratio, and uniformly mixing; s3: preparing three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon constructed by two-dimensional carbon nanosheets: and (3) transferring the reactant obtained in the step (S2) to a tubular furnace for reaction, and removing impurities to obtain the three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon constructed by the two-dimensional carbon nanosheets. The invention provides a universal path for preparing the heteroatom-doped carbon anode material for the zinc ion hybrid capacitor with the high area ratio capacitance.
Description
Technical Field
The invention relates to the technical field of carbon material preparation, in particular to a preparation method and application of three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon.
Background
For zinc ion hybrid capacitors, the performance is largely determined by the performance of the positive electrode material. The preparation method of the common carbon material is a template coupling strong base activation method, the method is easy to cause corrosion of equipment, strong acid is required to be used for neutralization in the post-treatment process, the cost is high, and the environment is polluted.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation method and application of three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon, the three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon constructed by two-dimensional carbon nanosheets for a zinc ion hybrid capacitor is prepared by a simple and environment-friendly process, and a universal path is provided for preparation of a heteroatom-doped carbon anode material for a high-area-ratio-capacitance zinc ion hybrid capacitor.
The invention provides a preparation method of three-dimensional nitrogen, phosphorus and sulfur doped honeycomb carbon, which comprises the following steps:
s1: preparation of Nitrogen and phosphorus precursors
Dissolving melamine in deionized water under the conditions of heating and stirring, then adding phytic acid, after reaction, freezing, filtering and drying to obtain a nitrogen source and a phosphorus source precursor;
s2: pretreatment of reactants
Grinding phenanthrene, potassium sulfate, potassium oxalate and nitrogen source and phosphorus source precursors in the S1 and uniformly mixing;
s3: preparation of three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon
And (3) transferring the reactant obtained in the step (S2) to a tubular furnace, reacting by taking argon as protective gas, and after the reaction is finished, cooling to room temperature and removing impurities to obtain the three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon constructed by the two-dimensional carbon nanosheets.
Preferably, the heating temperature in S1 is 60-80 ℃, and the reaction time is 6-12h.
Preferably, the molar ratio of the melamine to the phytic acid in the S1 is 1:1-3.
Preferably, the mass ratio of the phenanthrene, the potassium sulfate, the potassium oxalate, the nitrogen source and the phosphorus source precursor in S2 is 1.5-2:2-4.
Preferably, the reaction conditions in S3 are: argon flow is 3-12mL/min, temperature is 800-1000 ℃, and time is 30-150min.
The three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon prepared by the method provided by the invention.
The invention provides application of the three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon in a zinc ion hybrid capacitor.
Mechanism of action
The three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon constructed by the two-dimensional carbon nanosheets is synthesized in the confined space of potassium sulfate through the shearing action of potassium diacetate, wherein the potassium sulfate not only plays a role of a template, but also serves as a sulfur source to be doped with sulfur atoms. In addition, the melamine and phytic acid polymer not only can be used as a nitrogen source and a phosphorus source to introduce N, P heteroatom under the high temperature condition, but also can generate gas under the decomposition condition to play a physical activation role. The specific mechanism is as follows: firstly, phenanthrene molecules, potassium sulfate, potassium oxalate, melamine and phytic acid polymer are uniformly mixed in a solid state, the phenanthrene molecules are melted and coated on the surfaces of the potassium sulfate, potassium oxalate and melamine-phytic acid polymer in a heating process, and then the surfaces of the phenanthrene molecules are polymerized and carbonized. Along with the rise of the temperature, the potassium oxalate is decomposed to generate carbon dioxide gas, simultaneously, the carbon dioxide reacts with carbon to generate carbon monoxide, and the generated gas activates and forms pores on the surface of the carbon substrate to generate micropores for ion adsorption and mesopores for ion transmission of the electrolyte. In addition, a K simple substance generated by decomposition is embedded into a phenanthrene molecular layer after polymerization and carbonization, and a two-dimensional carbon nanosheet is synthesized under the synergistic shearing action of gas generated by reaction. And then, the carbon nano-sheets are connected with each other to form a three-dimensional honeycomb structure, and the honeycomb structure not only can be used as an electrolyte tank to store electrolyte ions, but also can be used as a channel for ion transmission. In addition, the melamine-phytic acid polymer is decomposed to generate gas containing N and P, and then the gas reacts with the carbon substrate to replace C element in the gas and introduce N, P heteroatom; meanwhile, potassium sulfate reacts with a carbon substrate to replace C atoms in the potassium sulfate, an S element is introduced, co-doping of N, P, S is achieved, and introduction of heteroatoms improves conductivity of the electrode material. And finally, repeatedly washing with water to remove impurities to obtain the three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon constructed by the two-dimensional carbon nanosheets.
Compared with the prior art, the invention has the beneficial technical effects
1. The invention takes potassium sulfate as a sulfur source and a template, and adopts a simple green and environment-friendly process to prepare the three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon constructed by two-dimensional carbon nano sheets for the zinc ion hybrid capacitor, thereby providing a general path for preparing the heteroatom-doped carbon anode material for the zinc ion hybrid capacitor with high area ratio capacitance;
2. according to the invention, by selecting the activating agent and the process, the use of strong alkali and strong acid substances is avoided, so that the risk of equipment corrosion is reduced, and the generation of subsequent waste liquid is reduced;
3. the product prepared by the invention has high specific surface area which reaches 2265.8m 2 /g；
4. When the product prepared by the invention is used as a positive electrode material of a zinc ion mixed capacitor, the product shows high area specific capacitance and large energy density.
Drawings
Fig. 1 is a nitrogen adsorption and desorption isotherm of three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon prepared from two-dimensional carbon nanosheets in embodiments 1, 2, and 3 of the present invention.
Fig. 2 is a field emission scanning electron microscope photograph of a three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon constructed by two-dimensional carbon nanosheets, prepared in embodiment 2 of the present invention.
Fig. 3 is an N1s diagram of three-dimensional nitrogen, phosphorus, and sulfur-doped honeycomb carbon constructed by two-dimensional carbon nanosheets, prepared in embodiment 2 of the present invention.
Fig. 4 is a P2P diagram of three-dimensional nitrogen phosphorus sulfur-doped honeycomb carbon constructed by two-dimensional carbon nanosheets, prepared in embodiment 2 of the present invention.
Fig. 5 is an S2p diagram of three-dimensional nitrogen phosphorus sulfur-doped honeycomb carbon constructed by two-dimensional carbon nanosheets, prepared in embodiment 2 of the present invention.
Fig. 6 is a graph of capacity of a zinc ion hybrid capacitor as a function of current density.
Fig. 7 is a graph of energy density as a function of power density for a zinc ion hybrid capacitor.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
The reagent is purchased from Aladdin Biotechnology Ltd, and the main instruments and equipment used in the preparation and characterization of the carbon material are as follows: a field emission scanning electron microscope (S-4800, hitachi corporation), an X-ray photoelectron diffractometer (Thermo EBCALAB250, sammerfei usa), a specific surface area adsorption apparatus (ASAP 2460, meike usa), a blue-ray battery test system (CT 3001A, knoop gmbh, wuhan), a tube furnace (OTF 1200X, mixcrystal materials technology ltd).
Example 1
The invention provides a specific preparation process of three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon constructed by two-dimensional carbon nanosheets, which comprises the following steps:
s1: preparation of nitrogen source and phosphorus source precursors: heating deionized water to 60 ℃, stirring at constant temperature, adding melamine, dissolving, slowly adding phytic acid, reacting for 6 hours, freezing, filtering and drying to obtain a nitrogen source and a phosphorus source precursor;
s2: pretreatment of reactants: grinding phenanthrene, potassium sulfate, oxalic acid and the product obtained in the step S1 according to a certain mass ratio, and uniformly mixing;
s3: and (3) transferring the reactant obtained in the step (S2) to a tubular furnace, reacting under the protection of argon, allowing the reactant to be cooled to room temperature, and removing impurities to obtain the three-dimensional nitrogen, phosphorus and sulfur doped honeycomb carbon constructed by the two-dimensional carbon nanosheets. Wherein the reaction condition is that the mixture is firstly heated to 98 ℃ at the speed of 2 ℃/min, the temperature is kept for 1h, then the mixture is heated to 850 ℃ at the speed of 5 ℃/min, and the mixture reacts for 30min at the temperature; the steps of removing impurities mainly comprise grinding, washing, drying, secondary grinding and sieving.
The molar ratio of the melamine to the phytic acid in the S1 is 1:1; s2, the mass ratio of phenanthrene, potassium sulfate, potassium oxalate, nitrogen source to phosphorus source precursor is 1.
The obtained three-dimensional honeycomb carbon constructed by two-dimensional carbon nano-sheets is named as NPS-HC 2 。
Example 2
The invention provides a specific preparation process of three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon constructed by two-dimensional carbon nanosheets, which comprises the following steps:
s1: preparation of nitrogen source and phosphorus source precursors: heating deionized water to 70 ℃, stirring at constant temperature, adding melamine, dissolving, slowly adding phytic acid, reacting for 9 hours, freezing, filtering and drying to obtain a nitrogen source and a phosphorus source precursor;
s2: pretreatment of reactants: grinding phenanthrene, potassium sulfate, an activating agent and the product obtained in the step S1 according to a certain mass ratio, and uniformly mixing;
s3: and (3) transferring the reactant obtained in the step (S2) to a tubular furnace, reacting under the protection of argon, allowing the reactant to be cooled to room temperature, and removing impurities to obtain the three-dimensional nitrogen, phosphorus and sulfur doped honeycomb carbon constructed by the two-dimensional carbon nanosheets. Wherein the reaction condition is that the mixture is firstly heated to 98 ℃ at the speed of 2 ℃/min, the temperature is kept for 1h, then the mixture is heated to 850 ℃ at the speed of 5 ℃/min, and the mixture reacts for 90min at the temperature; the steps of removing impurities mainly comprise grinding, washing, drying, secondary grinding and sieving.
In the S1, the molar ratio of melamine to phytic acid is 2; s2, the mass ratio of phenanthrene to potassium sulfate to potassium oxalate to the nitrogen source to the phosphorus source precursor is 1.2.
The obtained three-dimensional honeycomb carbon constructed by two-dimensional carbon nano-sheets is named as NPS-HC 3 。
Example 3
The invention provides a specific preparation process of three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon constructed by two-dimensional carbon nanosheets, which comprises the following steps:
s1: preparation of nitrogen source and phosphorus source precursors: heating deionized water to 80 ℃, stirring at constant temperature, adding melamine, dissolving, slowly adding phytic acid, reacting for 12 hours, freezing, filtering and drying to obtain a nitrogen source and a phosphorus source precursor;
s2: pretreatment of reactants: grinding phenanthrene, potassium sulfate, an activating agent and the product obtained in the step S1 according to a certain mass ratio, and uniformly mixing;
s3: and (3) transferring the reactant obtained in the step (S2) to a tubular furnace, reacting under the protection of argon, allowing the reactant to be cooled to room temperature, and removing impurities to obtain the three-dimensional nitrogen, phosphorus and sulfur doped honeycomb carbon constructed by the two-dimensional carbon nanosheets. Wherein the reaction condition is that the mixture is firstly heated to 98 ℃ at the speed of 2 ℃/min, the temperature is kept for 1h, then the mixture is heated to 900 ℃ at the speed of 5 ℃/min, and the mixture reacts for 150min at the temperature; the steps of removing impurities mainly comprise grinding, washing, drying, secondary grinding and sieving.
The mol ratio of melamine to phytic acid in the S1 is 3; s2, the mass ratio of phenanthrene to potassium sulfate to potassium oxalate to the nitrogen source to the phosphorus source precursor is 1.
The obtained three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon constructed by two-dimensional carbon nanosheets is named as NPS-HC 4 。
The products prepared in examples 1 to 3 were used as test samples to determine pore structure parameters and elemental composition and content, respectively. The results are shown in tables 1 and 2:
TABLE 1 pore structure parameters of three-dimensional nitrogen, phosphorus, and sulfur doped cellular carbon constructed from two-dimensional carbon nanosheets
As shown in Table 1 and the results in FIG. 1, the specific surface area of the carbon material prepared by the present invention is 1698.3-2265.8 m 2 The total pore volume is between 0.93 and 1.32cm 3 Between/g, and the interior contains abundant holes for storing and transmitting ions of the electrolyte, a honeycomb structure for conducting electrons and a large number of defect sites generated by nitrogen, phosphorus and sulfur heteroatoms for absorbing ions, and has a high specific surface area which reaches 2265.8m 2 /g。
Table 2 elemental composition and content of three-dimensional nitrogen phosphorus sulfur-doped honeycomb carbon constructed from two-dimensional carbon nanosheets
TABLE 2 As can be seen from FIGS. 2, 3, 4 and 5, NPS-HC 3 For example, the N, P, S content is 3.45%, 1.65%, 1.48%, respectively. In the preparation processThe potassium sulfate is used as a sulfur source and a template, the doping of nitrogen, phosphorus and sulfur elements in the three-dimensional carbon material matrix can be realized in the space of the limited area of the template, and a honeycomb structure with cavities is obtained in the carbon material matrix under the cutting action of an activator potassium diacetate, so that a large number of channels are provided for the transmission of ions and electrons.
The test method of FIG. 6 and FIG. 7 is to use zinc foil as the negative electrode, the prepared electrode material as the positive electrode, 3mol/LZn (CF) 3 SO 3 ) 2 The water solution is electrolyte, and the test voltage is 0.1-1.8V. Specific volume, energy density, and power density are calculated as C =2I ≧ Vdt/3.6Vm, E = I ≧ Vdt/3.6m, and P =3600E/t, respectively. The test results of examples 1-3 are shown in Table 3.
TABLE 3 Zinc ion hybrid capacitor Performance
As can be seen from fig. 6, fig. 7 and table 3, the carbon material prepared by the present invention shows high area capacity and large energy density when applied to a zinc ion capacitor.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. The preparation method of the three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon is characterized by comprising the following steps of:
s1: preparation of Nitrogen and phosphorus precursors
Dissolving melamine in deionized water under the conditions of heating and stirring, then adding phytic acid, after reaction, freezing, filtering and drying to obtain a nitrogen source and a phosphorus source precursor;
s2: pretreatment of reactants
Grinding phenanthrene, potassium sulfate, potassium oxalate and nitrogen source and phosphorus source precursors in the S1 and uniformly mixing;
s3: preparation of three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon
And (3) transferring the reactant obtained in the step (S2) to a tubular furnace, reacting by taking argon as protective gas, and after the reaction is finished, cooling to room temperature to remove impurities to obtain the three-dimensional nitrogen-phosphorus-sulfur-doped honeycomb carbon constructed by the two-dimensional carbon nanosheets.
2. The method for preparing the three-dimensional nitrogen phosphorus sulfur doped honeycomb carbon according to claim 1, wherein the heating temperature in the step S1 is 60-80 ℃, and the reaction time is 6-12h.
3. The method for preparing three-dimensional nitrogen phosphorus sulfur doped honeycomb carbon according to claim 1, wherein the molar ratio of melamine to phytic acid in S1 is 1:1-3.
4. The preparation method of the three-dimensional nitrogen phosphorus sulfur doped honeycomb carbon according to claim 1, wherein the mass ratio of phenanthrene, potassium sulfate, potassium oxalate, nitrogen source and phosphorus source precursor in S2 is 1.5-2:2-4.
5. The method for preparing the three-dimensional nitrogen phosphorus sulfur doped honeycomb carbon according to claim 1, wherein the reaction conditions in the step S3 are as follows: the flow rate of argon gas is 3-12mL/min, the temperature is 800-1000 ℃, and the time is 30-150min.
6. A three-dimensional nitrogen phosphorus sulfur doped carbon honeycomb prepared by the method of any one of claims 1 to 5.
7. Use of the three-dimensional nitrogen phosphorus sulfur doped honeycomb carbon of claim 6 in a zinc ion hybrid capacitor.
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