CN115124020A - Boron-nitrogen co-doped carbon material with hierarchical holes and preparation method and application thereof - Google Patents
Boron-nitrogen co-doped carbon material with hierarchical holes and preparation method and application thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
Abstract
The invention discloses a boron-nitrogen co-doped carbon material with hierarchical holes and a preparation method and application thereof, and belongs to the technical field of electrochemical energy storage materials. The invention relates to a preparation method of a boron-nitrogen co-doped carbon material with hierarchical pores, which is obtained by mixing ordered macroporous ZIF-8 serving as a carbon precursor with boric acid and performing heat treatment in an inert atmosphere; the preparation method comprises the following steps of taking regularly arranged polystyrene microspheres as a hard template, growing ZIF-8 in gaps of the polystyrene microspheres by an immersion method and a two-solvent initiation method, and finally etching the polystyrene microspheres by tetrahydrofuran to obtain the single-crystal ordered macroporous ZIF-8. The method can well control the pore distribution and porosity of the material, and improve the specific surface area and ion transmission capability of the material, so that the prepared boron-nitrogen co-doped carbon material with hierarchical pores has high electrochemical performance when being applied to a supercapacitor, and has wide application prospect.
Description
Technical Field
The invention relates to a boron-nitrogen co-doped carbon material with hierarchical pores and a preparation method and application thereof, belonging to the technical field of electrochemical energy storage materials.
Background
In recent years, environmental pollution and energy shortage have prompted continuous exploration for high-performance energy storage technologies. Among them, the super capacitor is receiving attention because of its advantages of fast charge and discharge rate, high power density, and long cycle life.
Compared with conductive polymers and metal oxides, the carbon material has the advantages of wide source, low cost, large specific surface area, excellent conductivity and the like, and gradually becomes an ideal electrode material of the super capacitor.
In order to optimize the energy storage performance of the supercapacitor, the carbon material should have the characteristics of large specific surface area, proper pore structure (including macropores, mesopores and micropores), abundant heteroatom doping and the like. The layered porous carbon structure is beneficial to the effective permeation of electrolyte into the material structure, improves the utilization rate of the specific surface area of the electrode material, shortens the ion diffusion path and further improves the electrochemical performance of the electrode material.
Specifically, macropores can be used for efficient storage of ions, mesopores facilitate diffusion of ions into the material body, and micropores facilitate adsorption of electrolyte ions. Among various carbon precursors, carbon materials derived from metal organic framework materials have the characteristics of controllable porosity, large specific surface area, various geometric shapes and the like, and are gradually applied to the fields of electrochemical energy storage and the like.
Zeolite imidazolate framework materials (ZIF-8) are metal organic framework materials with the characteristics of low cost and high nitrogen content, and can be directly prepared into nitrogen-doped porous carbon materials with excellent energy storage performance. However, the traditional method for constructing a porous structure cannot well control the pore distribution and porosity of the material, so that the electrochemical performance of the supercapacitor is poor.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a boron-nitrogen co-doped carbon material with hierarchical holes, which is low in preparation cost and excellent in performance, and a preparation method and application thereof. The boron-nitrogen co-doped carbon material with the hierarchical holes is obtained by mixing ordered macroporous ZIF-8 serving as a carbon precursor with boric acid and performing heat treatment in an inert atmosphere; the preparation method comprises the following steps of taking regularly arranged polystyrene microspheres as a hard template, growing ZIF-8 in gaps of the polystyrene microspheres by an immersion method and a double-solvent initiation method, and finally etching the polystyrene microspheres by tetrahydrofuran to obtain the monocrystal ordered macroporous ZIF-8.
The invention aims to provide a preparation method of a boron-nitrogen co-doped carbon material with hierarchical holes, which specifically comprises the following steps:
(1) mixing water, styrene and polyvinylpyrrolidone, adding a potassium persulfate aqueous solution, reacting at 60-80 ℃ for 18-36h, and then carrying out suction filtration and drying on a reaction solution to obtain a regularly arranged polystyrene microsphere template;
(2) soaking the regularly arranged polystyrene microsphere template obtained in the step (1) into a methanol solution containing zinc nitrate hexahydrate and 2-methylimidazole, standing, performing vacuum treatment on the template to ensure that the solution is fully soaked into gaps of the template, and taking out the template and drying;
(3) soaking the dried substance obtained in the step (2) into a mixed solution of methanol and ammonia water, carrying out vacuum treatment on the mixed solution, standing, and carrying out suction filtration and drying on the dried substance to obtain a dried substance;
(4) soaking the dried substance obtained in the step (3) in a tetrahydrofuran solution, standing, and then centrifuging, washing and drying the tetrahydrofuran solution to obtain ZIF-8 with a hierarchical pore structure;
(5) carrying out heat treatment on the ZIF-8 with the hierarchical pore structure prepared in the step (4) in an inert atmosphere to obtain a nitrogen-doped carbon material with the hierarchical pore structure;
(6) and (4) mixing the nitrogen-doped carbon material with the hierarchical pore structure prepared in the step (5) with boric acid, putting the mixture into a porcelain boat, and carrying out heat treatment in an inert atmosphere to obtain the boron-nitrogen co-doped carbon with the hierarchical pores.
In one embodiment of the present invention, the water used in step (1) is ultrapure water, and the amount used is 450-.
In one embodiment of the present invention, the ratio of styrene volume to polyvinylpyrrolidone in step (1) is 60 to 80: 0.12-0.14 mL/g.
In one embodiment of the present invention, the concentration of the aqueous potassium persulfate solution in the step (1) is from 0.5 to 5 wt%.
In one embodiment of the present invention, the mass ratio of zinc nitrate hexahydrate to 2-methylimidazole in step (2) is 23 to 26: 18-22.
In one embodiment of the invention, the mass ratio of the polystyrene microsphere template to the zinc nitrate hexahydrate in the step (2) is 1: 8-13.
In one embodiment of the present invention, the amount of the methanol solution in step (2) is 110-.
In one embodiment of the present invention, the standing time in step (2) is 0.5 to 2 hours.
In one embodiment of the present invention, the vacuum treatment time in step (2) is 0.5 to 2 hours; the drying temperature is 50-70 ℃.
In one embodiment of the present invention, the volume ratio of methanol to ammonia water in step (3) is 1.5:1 to 2.5: 1.
In one embodiment of the invention, the vacuum treatment time in the step (3) is 15-90min, the standing time is 18-36h, and the drying temperature is 50-70 ℃.
In one embodiment of the present invention, the standing time in step (4) is 20-48h, and the drying temperature is 100-120 ℃.
In one embodiment of the present invention, the inert atmosphere in step (5) is argon; the heat treatment temperature is 700-1000 ℃.
In one embodiment of the present invention, the mass ratio of the nitrogen-doped carbon material having a hierarchical pore structure to boric acid in step (6) is 1-7: 1-5.
In one embodiment of the present invention, the inert atmosphere in step (6) is argon, and the heat treatment temperature is 700-1000 ℃.
The second purpose of the invention is to provide a boron-nitrogen co-doped carbon material with graded pores prepared by the preparation method.
The third purpose of the invention is to provide an application of the boron-nitrogen co-doped carbon material with the hierarchical pores in preparing the super capacitor.
Compared with the prior art, the invention has the following remarkable advantages:
(1) in the structure taking ZIF-8 as a carbon precursor, macropores are introduced by a hard template method, and a hierarchical pore structure is obtained by annealing treatment, so that the specific surface area and the ion transmission capability of the material are improved;
(2) the boron element is introduced into the carbon skeleton, so that active sites on the surface of the carbon material are increased, the adsorption capacity on electrolyte ions is improved, and the hydrophilicity of the material is improved.
The invention combines a hierarchical porous structure and a double-heteroatom doping strategy, provides a new idea for the design of dodecahedron carbon, and can be used for not only water-based super capacitors, but also other energy storage devices.
Drawings
Fig. 1 is a schematic diagram of a process for preparing boron-nitrogen co-doped carbon with graded holes in example 1 of the present invention;
fig. 2 is an SEM image of boron-nitrogen co-doped carbon with graded pores prepared in example 1 of the present invention;
FIG. 3 is an EDS diagram of boron-nitrogen co-doped carbon with graded pores prepared in example 1 of the present invention;
FIG. 4 is a graph showing electrochemical properties of supercapacitors of the carbon materials prepared in example 1, comparative example 2 and comparative example 3;
FIG. 5 is a graph showing the electrochemical performance of a boron-nitrogen-co-doped carbon supercapacitor with graded pores prepared in example 1 of the present invention;
fig. 6 is an SEM image of the material prepared in comparative example 4.
Detailed Description
The invention will now be further illustrated by reference to specific examples, which are intended to be illustrative only and not to limit the scope of the invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
1. Electrochemical test method: adopting a three-electrode test system, taking the prepared boron-nitrogen co-doped carbon with hierarchical holes as a working electrode, an Ag/AgCl electrode as a reference electrode, a graphite rod as a counter electrode, and 1mol/L electrolyte H 2 SO 4 A solution; the electrochemical performance of the material prepared by the method is researched by adopting a conventional electrochemical testing means.
The mass specific capacitance (C) of the electrode material can be obtained from the charge-discharge curve s ) The concrete formula is as follows:
wherein, C s For mass specific capacitance, I is the current, Δ t is the discharge time, m is the electrode active material mass, and V is the potential window.
Example 1
A preparation method of a boron-nitrogen co-doped carbon material with hierarchical holes specifically comprises the following steps:
(1) mixing 500mL of water, 75mL of styrene and 0.125g of polyvinylpyrrolidone, adding 50mL of potassium persulfate aqueous solution, reacting at 75 ℃ for 24 hours, and carrying out suction filtration and drying on reaction liquid to obtain a regularly-arranged polystyrene microsphere template;
(2) soaking the regularly arranged polystyrene microsphere template prepared in the step (1) into 135mL of methanol solution containing 24.45g of zinc nitrate hexahydrate and 20.25g of 2-methylimidazole, standing for 1h, then carrying out vacuum treatment on the solution to ensure that the solution is fully soaked in gaps of the template, and then taking out the template and drying the template at the temperature of 60 ℃; obtaining the treated polystyrene microsphere template;
(3) soaking the polystyrene microsphere template treated in the step (2) into a mixed solution of methanol and ammonia water (volume ratio is 2:1), standing for 24h, then carrying out suction filtration on the obtained product, and drying filter residues at 60 ℃;
(4) soaking the dried substance obtained in the step (3) in a tetrahydrofuran solution, standing for 24h, centrifuging, washing, and drying at 110 ℃ to obtain a ZIF-8 material with a hierarchical pore structure;
(5) carrying out high-temperature heat treatment on the ZIF-8 material obtained in the step (4) in an inert atmosphere of argon at 900 ℃ for 1h to obtain a nitrogen-doped carbon material with a hierarchical pore structure, which is marked as N-HPC;
(6) and (3) mixing the nitrogen-doped carbon material with the hierarchical pore structure obtained in the step (5) with boric acid (the mass ratio is 4: 1), putting the mixture into a porcelain boat, and carrying out high-temperature heat treatment in an inert atmosphere of argon at the temperature of 900 ℃ for 1h to obtain the boron-nitrogen co-doped carbon material with the hierarchical pores, which is recorded as BN-HPC. FIG. 1 is a schematic diagram of a preparation process of boron-nitrogen co-doped carbon with graded pores.
Comparative example 1
The difference from example 1 is that step (6) was omitted and the N-HPC material was obtained directly.
Comparative example 2
The boric acid in step (6) of example 1 was replaced with an equimolar amount of diphenyl sulfide, and after stirring at 85 ℃ for 12 hours, it was dried by centrifugation. And (3) putting the dried material into a porcelain boat, and carrying out high-temperature heat treatment under the inert atmosphere of argon at 900 ℃ for 1h to obtain the sulfur-nitrogen co-doped carbon material with the graded holes, wherein the obtained material is marked as SN-HPC.
Comparative example 3
N-HPC was immersed in an equimolar phosphoric acid solution, stirred at 85 ℃ for 12 hours, and then dried by centrifugation. And (3) putting the dried material into a porcelain boat, and carrying out high-temperature heat treatment under the inert atmosphere of argon at 900 ℃ for 1h to obtain the phosphorus-nitrogen co-doped carbon material with graded holes, which is recorded as PN-HPC.
Comparative example 4
And (4) mixing boric acid with the ZIF-8 material with the hierarchical pore structure obtained in the step (4), and performing high-temperature heat treatment in an inert atmosphere of argon. The remaining operating parameters were consistent with those of example 1, and as a result, the pore structure of the resulting carbon material collapsed and the morphology was destroyed, as shown in FIG. 6.
Comparative example 5
In the preliminary experiment process of the present invention, the mass ratios of the nitrogen-doped carbon material of the hierarchical pore structure and boric acid were set to 7:1, 4:1, 1:1, 1:4, respectively, and the remaining operational parameters were the same as in the step of example 1. And carrying out electrochemical test on the obtained material, wherein the test charging and discharging time shows a trend of increasing and then decreasing along with the increase of the content ratio of boric acid, and only when the mass ratio of the nitrogen-doped carbon material to the boric acid is 4:1, the specific capacity performance of the material is optimal.
Material characterization and Performance testing
1. The structural morphology and the element distribution of the boron-nitrogen co-doped carbon with the hierarchical holes obtained in the embodiment are characterized by using a Scanning Electron Microscope (SEM), an X-ray Energy Dispersion Spectrum (EDS) and an electrochemical workstation; the results are as follows:
(1) as shown in fig. 2, SEM test results show that the prepared boron-nitrogen co-doped carbon with hierarchical pores is a polyhedral material with regular pore structure, and the size of the pores is about 170 nm. In addition, the surface of the material is not smooth because the material has a microporous structure due to the annealing treatment.
(2) As shown in fig. 3, the EDS test results show that the boron element, the nitrogen element and the carbon element are uniformly distributed in the boron-nitrogen co-doped carbon with graded pores, which proves the successful doping of the boron and the nitrogen element.
2. And (3) electrochemical performance testing:
as shown in fig. 4, electrochemical test results show that the boron-nitrogen co-doped carbon with graded pores prepared in example 1 has longer discharge time, more excellent electrochemical performance and current density of 10Ag, compared with other materials -1 When the specific capacitance is 183.3F g -1 Greater than the specific capacitance of other materials; wherein, the SN-HPC specific capacitance of comparative example 2 is 168.9F g -1 (ii) a The specific PN-HPC capacitance of comparative example 3 is 164.4F g -1 (ii) a Comparative example 1 has a specific N-HPC capacity of 161.1F g -1 . Experimental results prove that the electrochemical performance of the heteroatom double-doped carbon material is superior to that of a single-doped carbon material, and the boron-nitrogen-doped carbon material has more excellent performance in the double-doped carbon material.
As shown in FIG. 5, the results of electrochemical tests showed that the BN-HPC-electrode well maintained its symmetrical triangular shape even at high scan rate/current density, indicating that the BN-HPC-electrode has good rate stability and excellent electrochemical energy storage performance at a current density of 1Ag -1 When the specific capacitance is 236.9F g -1 。
Claims (10)
1. A preparation method of a boron-nitrogen co-doped carbon material with hierarchical pores is characterized by comprising the following steps:
(1) mixing water, styrene and polyvinylpyrrolidone, adding a potassium persulfate aqueous solution, reacting at 60-80 ℃ for 18-36h, and then carrying out suction filtration and drying on a reaction solution to obtain a regularly arranged polystyrene microsphere template;
(2) soaking the regularly arranged polystyrene microsphere template obtained in the step (1) into a methanol solution containing zinc nitrate hexahydrate and 2-methylimidazole, standing, performing vacuum treatment on the template to ensure that the solution is fully soaked into gaps of the template, and taking out the template and drying;
(3) soaking the dried substance obtained in the step (2) into a mixed solution of methanol and ammonia water, carrying out vacuum treatment on the mixed solution, standing, and carrying out suction filtration and drying on the dried substance to obtain a dried substance;
(4) soaking the dried substance obtained in the step (3) in a tetrahydrofuran solution, standing, and then centrifuging, washing and drying the solution to obtain ZIF-8 with a hierarchical pore structure;
(5) carrying out heat treatment on the ZIF-8 with the hierarchical pore structure prepared in the step (4) in an inert atmosphere to obtain a nitrogen-doped carbon material with the hierarchical pore structure;
(6) and (4) mixing the nitrogen-doped carbon material with the hierarchical pore structure prepared in the step (5) with boric acid, putting the mixture into a porcelain boat, and carrying out heat treatment in an inert atmosphere.
2. The preparation method according to claim 1, wherein the ratio of the volume of the styrene to the mass of the polyvinylpyrrolidone in the step (1) is 60-80: 0.12-0.14 mL/g.
3. The production method according to claim 1, wherein the concentration of the aqueous potassium persulfate solution in the step (1) is from 0.5 to 5% by weight.
4. The preparation method according to claim 1, wherein the mass ratio of zinc nitrate hexahydrate to 2-methylimidazole in step (2) is 23-26: 18-22.
5. The preparation method according to claim 1, wherein the mass ratio of the polystyrene microsphere template to the zinc nitrate hexahydrate in the step (2) is 1: 8-13.
6. The method according to claim 1, wherein the vacuum treatment time in the step (2) is 0.5 to 2 hours; the drying temperature is 50-70 ℃.
7. The method according to claim 1, wherein the inert atmosphere in the step (5) is argon; the heat treatment temperature is 700-1000 ℃.
8. The production method according to claim 1, wherein the mass ratio of the nitrogen-doped carbon material having a hierarchical pore structure to boric acid in step (6) is 1-7: 1-5.
9. The boron-nitrogen co-doped carbon material with graded pores prepared by the preparation method of any one of claims 1 to 8.
10. Use of the boron-nitrogen co-doped carbon material with graded pores according to claim 9 in preparation of a supercapacitor.
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