CN108455559B - BN bond breaking-based nitrogen-boron co-doped porous carbon material and preparation method and application thereof - Google Patents
BN bond breaking-based nitrogen-boron co-doped porous carbon material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a BN bond breaking based nitrogen and boron co-doped porous carbon material which is prepared by carrying out hydrothermal reaction on resorcinol, formaldehyde and boron nitride under an alkaline condition to obtain nitrogen-containing gel, carrying out freeze drying, grinding treatment on an alkaline inorganic substance, carbonizing, washing and drying, wherein the specific surface area range of the nitrogen-containing gel is 1000-1200 m2g‑1. The preparation method comprises the following steps: 1) preparing a nitrogen-containing gel; 2) drying the nitrogen-containing gel; 3) activating the nitrogen-containing gel; 4) carbonizing the nitrogen-containing gel; 5) and (3) preparing the nitrogen and boron co-doped porous carbon material based on breaking BN bond. The super capacitor electrode material is applied, the current density is 20-0.5A/g, and the specific capacitance reaches 150.0-250.0F/g. Compared with the prior art in which the nitrogen source and the boron source are doped in two steps, the method has the most outstanding advantages that the nitrogen source and the boron source are doped in one step, a stable BN bond is simply broken, the production efficiency is greatly improved, the cost is reduced, and the method has wide application prospects in the field of supercapacitors.
Description
Technical Field
The invention belongs to the field of electrochemical super capacitors, and particularly relates to a BN bond breaking based nitrogen and boron co-doped porous carbon material.
Background
With the rapid growth of population and the rapid development of economy, the gradual shortage of resources and energy sources becomes one of the important problems to be solved urgently in contemporary society. Therefore, the development and application of clean and renewable energy sources play a key role in the national economic development and the solution of environmental problems. Electric energy, wind energy, solar energy, tidal energy and the like are widely concerned, and finding a proper energy storage device is a crucial link.
The super capacitor is a novel energy storage device between a traditional capacitor and a rechargeable battery, has the advantages of high power density, long cycle life, high charging and discharging speed, wide use temperature range, no pollution to the environment and the like, and is applied to the fields of electric automobiles, aerospace, national defense science and technology and the like. The materials of the super capacitor are mainly divided into three types: carbon materials, conductive polymers, and metal oxides. The carbon material has the advantages of large specific surface area, low cost, good conductivity and the like. The surface of the pure carbon material is hydrophobic, so that the contact resistance between electrolyte ions and holes is greatly improved, the capacitance characteristic is influenced, the carbon material can only form double-layer capacitance which is nearly 100 times lower than pseudo capacitance, functional groups can be introduced into the surface of the carbon material by doping nitrogen, the surface wettability of the carbon material can be improved, the conductivity is greatly improved, the specific surface area and the specific capacitance of the electrode material can be improved by doping boron, and therefore, the nitrogen and boron co-doped porous carbon attracts great attention as the electrode material.
The phenolic resin is low in price, good in conductivity, simple and convenient in synthesis process and has a porous structure, so that the phenolic resin attracts attention, and the conductivity and the capacitance of the phenolic resin can be improved by introducing a nitrogen source and a boron source into the phenolic resin. However, the prior art, chinese patent CN201310293898.1, discloses that the nitrogen source and boron source are introduced separately by different compounds; the article "Boron and nitrogen co-seeded porous carbon with a high concentration of Boron and its super particulate catalyst" discloses that the nitrogen source and the Boron source are not only introduced separately but are introduced completely by a two-step experiment.
Therefore, the prior art has the technical problems of complicated preparation process and long time consumption caused by the fact that nitrogen and boron cannot be added simultaneously. Therefore, how to introduce a nitrogen source and a boron source to improve the performance of the porous carbon with high efficiency and simplicity becomes a focus of attention of extensive researchers.
Disclosure of Invention
The invention aims to provide a BN bond breaking based nitrogen and boron co-doped porous carbon material and a preparation method and application thereof. The nitrogen element and the boron element are doped into the phenolic resin step by step, so that the synthetic process of the nitrogen-boron co-doped porous carbon is greatly simplified.
Since the BN bond in boron nitride is very strong, it is difficult to break even when heated to 1000 ℃ or higher. Therefore, when boron nitride is directly incorporated into a phenol resin, the BN bond in the boron nitride is not broken and the boron nitride is not carbonized. Therefore, the effect of nitrogen boron co-doping cannot be achieved.
According to the invention, by adding an alkaline substance such as potassium hydroxide or sodium hydroxide, BN (boron nitride) bonds in boron nitride are broken under an alkaline condition, so that the boron nitride is completely carbonized, and finally nitrogen atoms and boron atoms can be doped into a carbon material separately, so that the technical effect of nitrogen and boron co-doping of porous carbon is achieved.
Compared with the rest of nitrogen and boron co-doped porous carbon, the method disclosed by the invention has the advantages that the nitrogen element and the boron element are doped into the porous carbon in a one-step manner, the electron transmission mechanism is improved, and the electrode material with high specific capacitance and low cost is obtained.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that:
a nitrogen and boron co-doped porous carbon material based on breaking BN bonds is prepared by stirring resorcinol, formaldehyde and boron nitride at normal temperature under an alkaline condition, performing hydrothermal reaction to obtain nitrogen and boron co-doped gel, performing freeze drying, activating treatment on an alkaline inorganic substance, carbonizing, washing and drying, wherein the specific surface area of the nitrogen-doped porous carbon material ranges from 1000 m to 1200 m2g-1。
The preparation method of the BN bond breaking based nitrogen and boron co-doped porous carbon material comprises the following steps:
step 1) preparation of nitrogen and boron co-doped gel, wherein sodium hydroxide, resorcinol, formaldehyde and boron nitride are mixed according to the mass ratio of 0.02:1:2: (0-3) stirring the solution at normal temperature for 3-5 hours to obtain nitrogen and boron co-doped gel;
step 2), drying the nitrogen-boron co-doped gel, namely performing freeze drying on the nitrogen-boron co-doped gel at the temperature of-40 to 50 ℃ for 40 to 50 hours to obtain a dried nitrogen-boron co-doped precursor;
step 3) activating the nitrogen-boron co-doped gel, mixing a dry nitrogen-boron co-doped precursor with an alkaline substance according to a mass ratio of 1 (1-3), and stirring at normal temperature for 0.1-1 hour to obtain an activated nitrogen-boron co-doped precursor, wherein the alkaline substance is potassium hydroxide or sodium hydroxide;
step 4), carbonizing the nitrogen and boron co-doped gel, putting the activated nitrogen and boron co-doped precursor into a tubular furnace, and calcining at 550-650 ℃ at a speed of 4-6 ℃/min for 2-4 h in a nitrogen atmosphere to obtain the carbonized nitrogen and boron co-doped gel;
and step 5) preparing the nitrogen and boron co-doped porous carbon material based on breaking of the BN bond, repeatedly washing the carbonized nitrogen and boron co-doped gel for 3-5 times by using 1mol/L hydrochloric acid solution and deionized water, and drying for 10-20 hours at the temperature of 80-90 ℃ to obtain the nitrogen and boron co-doped porous carbon material based on breaking of the BN bond.
Based on the application of the BN bond breaking nitrogen-boron co-doped porous carbon material as the electrode material of the supercapacitor, the current density is 20-0.5A/g, and the specific capacitance reaches 150.0-250.0F/g.
The invention is tested by a American (Quantachrome Instruments) Autosorb-1 type physical adsorption instrument and an IVIUM electrochemical workstation in the Netherlands, and the following results show that: according to the invention, the specific surface area of the nitrogen-boron co-doped porous carbon material based on breaking of BN bond is 1000-1200 m2g-1。
When the BN bond breaking nitrogen-boron co-doped porous carbon material is applied as a supercapacitor electrode material, the current density is 20-0.5A/g, and the specific capacitance reaches 150-250F/g.
According to the invention, the cyclic voltammetry test result of the nitrogen-boron co-doped porous carbon material based on breaking of BN bonds shows that under different scanning rates, the cyclic voltammetry curve keeps a good rectangular shape, and has good double-electric-layer capacitance behavior and electrochemical reversibility.
According to the invention, a typical carbon material curve is shown based on an XRD (X-ray diffraction) pattern of the boron-nitrogen co-doped porous carbon material for breaking BN (boron nitride) bonds, steamed bun peaks appear at 24.3 and 43.84 degrees respectively, which proves that the good graphitization degree is achieved, and the NB bonds are broken and boron nitride is carbonized.
The XPS spectrum of the nitrogen and boron co-doped porous carbon material for breaking BN bonds shows characteristic peaks of C, O, N and B, and indicates that the material contains C, O, N and B elements, thereby indicating the successful doping of the nitrogen element and the boron element.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the new boron nitride source is utilized, so that the nitrogen source and the boron source can be doped in one step, compared with the prior boron-nitrogen co-doping process (the boron and the nitrogen source are doped in two steps), the doping process is greatly simplified, and the nitrogen element and the boron element are effectively doped.
2. The specific capacitance of the electrolyte in an aqueous electrolyte (6M KOH solution) is high, and is 150-250F/g at 20-0.5A/g.
3. Under the condition of low temperature, the stable BN bond is broken through adding alkaline substances, the nitrogen element and the boron element are doped into the phenolic resin step by step, and the nitrogen and boron co-doping synthesis process is greatly simplified.
Therefore, the invention keeps the high specific capacitance of the electrode material and has good rate performance under the conditions of reducing the synthesis process and adopting the one-step doping of the nitrogen source and the boron source.
Description of the drawings:
fig. 1 is a cyclic voltammetry curve of a supercapacitor of a three-electrode system assembled by a nitrogen-boron co-doped porous carbon material activated by potassium hydroxide and based on breaking BN bonds, prepared in the example of the invention;
fig. 2 is a charge-discharge cycle performance curve of a supercapacitor of a three-electrode system assembled by a nitrogen-boron co-doped porous carbon material activated by potassium hydroxide and based on breaking a BN bond, which is prepared in an embodiment of the present invention, at different current densities;
FIG. 3 is an adsorption-desorption isotherm of a BN bond breaking-based nitrogen-boron co-doped porous carbon material activated by potassium hydroxide prepared in the example of the invention;
FIG. 4 is an XRD (X-ray diffraction) spectrum of the BN bond breaking-based nitrogen-boron co-doped porous carbon material activated by potassium hydroxide and prepared in the embodiment of the invention;
FIG. 5 is an XRD (X-ray diffraction) pattern of a BN bond breaking based nitrogen and boron co-doped porous carbon material which is not activated by potassium hydroxide and is prepared in the embodiment of the invention;
FIG. 6 is an XPS spectrum of a BN bond-breaking nitrogen and boron co-doped porous carbon material activated by potassium hydroxide and prepared in an example of the invention;
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings, which are given by way of examples, but are not intended to limit the present invention.
Examples
A preparation method of a nitrogen and boron co-doped porous carbon material based on breaking of BN bonds comprises the following steps:
step 1) mixing sodium hydroxide, resorcinol, formaldehyde and boron nitride according to a mass ratio of 0.02:1:2:3, weighing 0.02g of sodium hydroxide, 2.2g of resorcinol, 4.4g of formaldehyde and 3g of boron nitride to prepare a solution, stirring at normal temperature for 4 hours, and carrying out hydrothermal reaction at 160 ℃ for 24 hours to obtain nitrogen-containing boron gel;
step 2) freeze-drying the nitrogen-boron-containing gel at-40 ℃ for 48 hours to obtain a dried nitrogen-boron-containing gel;
step 3) mixing the dried nitrogen-containing gel with an alkaline inorganic substance potassium hydroxide according to the mass ratio of 1:2, adding a proper amount of distilled water, and grinding at normal temperature for 0.5 hour to obtain activated nitrogen-doped boron porous carbon;
step 4), carbonizing the nitrogen-doped boron precursor in a nitrogen atmosphere, raising the temperature to 600 ℃ at a speed of 5 ℃/min, keeping the temperature for 3 hours, and cooling to room temperature to obtain a carbonized nitrogen-doped boron porous carbon material;
and 5) cleaning the nitrogen and boron co-doped porous carbon material subjected to 4 times of carbonization by using 1mol/L hydrochloric acid solution and deionized water, putting the sample into an oven at 85 ℃, and drying for 12 hours to obtain the BN bond breaking nitrogen and boron co-doped porous carbon material.
To demonstrate that the addition of potassium hydroxide breaks BN bonds and thereby fully carbonizes the boron nitride-added phenolic resin, and also introduces a nitrogen source and a boron source, an example was prepared for comparison that was not activated with potassium hydroxide, with the same steps as the above example, except that:
the step 1) is to obtain nitrogen-boron-containing gel;
the step 2) is to obtain dry gel containing nitrogen and boron;
activating with potassium hydroxide to obtain a precursor containing nitrogen and boron without activation in the step 3);
the carbonized porous carbon material containing nitrogen and boron is obtained in the step 4);
and 5) obtaining the porous carbon material containing nitrogen and boron.
The cyclic voltammetry test of the BN bond breaking based nitrogen and boron co-doped porous carbon material activated by potassium hydroxide prepared in the above example shows that the cyclic voltammetry curve keeps good rectangular shape under different scanning rates, and has good electric double layer capacitance behavior and electrochemical reversibility, as shown in FIG. 1.
The nitrogen and boron co-doped porous carbon material activated by potassium hydroxide and based on breaking BN bonds prepared in the example has the test result that the specific capacitance is 237F/g when the current density is 0.5A/g as shown in figure 2; when the current density is 20A/g, the specific capacitance is 178.0F/g respectively, and the rate performance is good.
Test results of preparing nitrogen and boron co-doped porous carbon material activated by potassium hydroxide and based on breaking BN bond are shown in FIG. 3, and the specific surface area of the material is 1014 m2 g-1。
The XRD pattern of the boron-nitrogen co-doping based on breaking BN bonds prepared without potassium hydroxide activation is shown in fig. 4, and the pattern is consistent with that of boron nitride, indicating that the structure of boron nitride is not broken.
The XRD pattern of the boron-nitrogen co-doping based on breaking BN bonds activated by potassium hydroxide prepared in example is shown in fig. 5, which shows a characteristic pattern of a carbon material, indicating that the molecular covalent bonds of boron nitride after grinding with potassium hydroxide are broken and boron nitride is carbonized.
The XPS spectrum of the BN bond breaking based nitrogen and boron codoped material activated by potassium hydroxide prepared in the example is shown in FIG. 6, and characteristic peaks of C, O, N and B can be seen, which indicates that the electrode material contains four elements of C, O, N and B, and nitrogen and boron are successfully doped into phenolic resin.
Claims (1)
1. A preparation method of a nitrogen and boron co-doped porous carbon material based on BN bond breaking is characterized by comprising the following steps:
step 1) preparing nitrogen and boron codoped gel, namely preparing sodium hydroxide, resorcinol, formaldehyde and boron nitride into a solution according to a certain mass ratio, stirring at normal temperature, and carrying out hydrothermal reaction to obtain nitrogen and boron containing gel;
the mass ratio of sodium hydroxide, resorcinol, formaldehyde and boron nitride in the step 1) is 0.02:1:2:3, after stirring for 3-5 hours at normal temperature in the step 1), carrying out hydrothermal reaction for 20-30 hours at 150-180 ℃;
step 2), drying the nitrogen and boron co-doped gel, and freeze-drying the nitrogen and boron co-doped gel to obtain a dried nitrogen and boron co-doped precursor;
the freeze drying conditions in the step 2) are that the freezing temperature is minus 40-50 ℃, and the drying time is 40-50 hours;
step 3), activating the nitrogen and boron co-doped gel, mixing a dry nitrogen and boron co-doped precursor and an alkaline substance according to a certain mass ratio, and activating under a certain condition to obtain an activated nitrogen and boron co-doped precursor;
the step 3) of nitrogen and boron co-doping the precursor: the mass ratio of the sodium hydroxide is 1 (1-3), the activation condition of the step 3) is grinding for 0.1-1 hour at normal temperature, and the alkaline substance of the step 3) is sodium hydroxide;
step 4), carbonizing the nitrogen and boron co-doped gel, putting the activated nitrogen and boron co-doped precursor into a tubular furnace, and calcining under a certain condition to obtain the carbonized nitrogen and boron co-doped gel;
the carbonization condition in the step 4) is that the carbonization is carried out for 2-4 h by raising the temperature to 550-650 ℃ at 4-6 ℃/min under the nitrogen atmosphere;
step 5) preparing a nitrogen and boron co-doped porous carbon material based on breaking of BN bonds, washing and drying the carbonized nitrogen and boron co-doped gel under certain conditions to obtain the nitrogen and boron co-doped porous carbon material based on the phenolic resin;
the washing and drying conditions in the step 5) are that 1mol/L hydrochloric acid solution and deionized water are repeatedly washed for 3-5 times, and then dried for 10-20 hours at the temperature of 80-90 ℃;
the specific surface area of the nitrogen-doped boron porous carbon material is 1000-1200 m2g-1。
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