CN113838676A - Velvet-interwoven spheroidal carbon-nitrogen-doped CaTi2O4(OH)2Preparation method of porous nano material - Google Patents
Velvet-interwoven spheroidal carbon-nitrogen-doped CaTi2O4(OH)2Preparation method of porous nano material Download PDFInfo
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 30
- 239000007772 electrode material Substances 0.000 claims abstract description 29
- 238000002360 preparation method Methods 0.000 claims abstract description 27
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- 239000002243 precursor Substances 0.000 claims abstract description 21
- 239000003990 capacitor Substances 0.000 claims abstract description 9
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
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- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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Abstract
The invention discloses a down feather interweaving sphere-like carbon and nitrogen doped CaTi2O4(OH)2The preparation method of the porous nano material comprises the steps of firstly preparing CaTi2O4(OH)2The precursor solution is combined with non-carbonized feathers, and the porous nano-particles with excellent electrochemical performance and serving as the electrode material of the super capacitor are obtained by adopting the solvothermal process with simple operation and low costRice material. In addition, the velvet interweaved spheroidal carbon-nitrogen-doped CaTi is also disclosed2O4(OH)2The product prepared by the preparation method of the porous nano material and the application thereof. The invention well keeps the microstructure of the feather, not only improves the pore structure distribution, but also enables the feather to have larger specific surface area, and the obtained porous nano material has good dispersibility and more excellent electrochemical performance.
Description
Technical Field
The invention relates to the technical field of porous nano materials, in particular to carbon and nitrogen doped CaTi2O4(OH)2A preparation method of the porous nano material, a product and application thereof.
Background
Along with the problems of global energy shortage, environmental pollution and the like, the demand for better energy storage materials is more and more urgent. Electric energy is indispensable convenient and cleanest energy in modern society, and is the main power for scientific and technical development and national economy leap. The energy storage discipline is used as a new field of multidisciplinary cross fusion of new energy, new materials and the like, and plays a vital role in promoting energy revolution and new energy state development. The super capacitor is used as an energy storage device capable of being charged and discharged quickly, and has the characteristics of high power density, short charging and discharging time, long service life, good temperature characteristic, energy conservation, environmental protection and the like. Electrochemical properties of the super capacitor mainly comprise capacitance, energy density, power density, cycling stability and the like, and the selection of electrode materials has very important influence on the electrochemical properties. The performance of the electrode material is closely related to the specific surface area, electrochemical activity, conductivity, stability and the like of the electrode material. Therefore, the preparation of the electrode is the key for improving the electrochemical performance of the supercapacitor.
On the basis of earlier stage experiments, the inventor of the application adopts a solvothermal method to obtain pure metastable phase CaTi2O4(OH)2The nano structure has better electrochemical performance, meets the charge storage mechanism of the Faraday pseudo capacitor, has simple preparation process and low cost, but is pure CaTi2O4(OH)2The nano sheet has poor conductivity, and the charging and discharging curves are not symmetrical enough, so the cycling stability is poor. For this reason, research was also conductedThe specific surface area is up to 600m2CaTi in g2O4(OH)2Although the honeycomb powder has a large specific surface area, the pore size distribution is large (80-165 nm), and the electrochemical performance is poor. Therefore, it is worth exploring how to improve the problems of poor conductivity and the like while maintaining a large specific surface area and a proper pore size.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a velvet interweaved spheroidal carbon-nitrogen-doped CaTi2O4(OH)2The preparation method of the porous nano material adopts solvothermal technology to obtain the porous nano material which has excellent electrochemical performance and is used as the electrode material of the super capacitor with simple operation and low cost. Another object of the present invention is to provide a method for producing a fiber-reinforced composite material using the above-mentioned down-feather-interlaced spheroidal carbon-nitrogen-doped CaTi2O4(OH)2The product prepared by the preparation method of the porous nano material and the application thereof.
The purpose of the invention is realized by the following technical scheme:
the invention provides a down feather interweaving spheroidal carbon and nitrogen doped CaTi2O4(OH)2The preparation method of the porous nano material comprises the following steps:
(1) disinfecting, washing and drying the feathers to obtain pretreated feathers;
(2) dissolving tetra-n-butyl titanate in ethanol according to a molar ratio of 1: 7.5-8.5, and stirring and mixing to obtain a solution A;
(3) dissolving anhydrous calcium chloride into distilled water according to the molar ratio of 5-25: 300-500: 10-20 of calcium chloride to distilled water to ethanol, adding ethanol, and stirring and mixing to obtain a solution B;
(4) adding the solution A into the solution B according to the molar ratio of calcium chloride to tetra-n-butyl titanate of 1: 1-2, stirring and mixing for the first time, adding an alkaline solution to adjust the pH value to 7.5-8.5, and continuously stirring and mixing for the second time to obtain CaTi2O4(OH)2A precursor;
(5) according toMass ratio of CaTi2O4(OH)2Stirring and mixing the precursor and the pretreated feather at the ratio of 1: 0.1-1.2, putting the mixture into a hydrothermal reaction kettle, preserving the heat for 18-30 hours at the hydrothermal temperature of 160-200 ℃, washing, filtering and drying a reaction product to obtain the feather interwoven spheroidal carbon and nitrogen doped CaTi2O4(OH)2A porous nanomaterial.
The inventor of the application finds that carbon and nitrogen doping is one of effective methods for improving the performance of the electrode, the carbon and nitrogen doping can increase the roughness and the hydrophilicity of the surface and enhance the adsorption effect of the surface of the electrode, and the N-containing functional group provides more active sites for the surface of the electrode and can form a micropore and mesopore structure to facilitate the rapid transmission of ions. The feather is a natural product, inherits C, N, P, S element naturally, has obvious fine keratin filaments, and can generate a high-activity carbon-nitrogen-doped porous structure under proper treatment. Therefore, in order to develop an electrode material with excellent comprehensive performance, the feather is used as a nitrogen source and a carbon source and is doped into CaTi by a solvothermal method2O4(OH)2Thereby preparing the electrode material with adjustable pore size distribution, stable electrochemical performance, high specific capacitance and excellent rate performance.
Further, in the step (1), the feather is soaked in a chlorine dioxide solution for 18-24 hours for disinfection, then the disinfected feather is washed with distilled water for 5-10 times, then soaked in an ethanol solution for 1-2 days for secondary disinfection and subjected to ultrasonic oscillation for 30min, then washed with distilled water for 5-10 times, and the feather is placed in a ventilated place for natural drying to obtain the pretreated feather. Wherein, the weight ratio of the feather to the chlorine dioxide solution to the distilled water to the ethanol is 1-20: 1-5: 500-2000: 5-50.
In the scheme, the feather is bird feather, such as chicken feather, pigeon feather, duck feather, goose feather and the like.
Further, the alkaline solution in the preparation method of the invention is one or a combination of a sodium hydroxide solution, ammonia water and a potassium hydroxide solution. The stirring and mixing time of the step (2) is 5-10 min; the stirring and mixing time of the step (3) is 5-10 min; the primary stirring and mixing time of the step (4) is 10-20 min, and the secondary stirring and mixing time is 15-35 min; and (5) stirring and mixing for 5-20 min. The drying in the step (5) is vacuum drying or freeze drying, wherein the vacuum drying is drying for 24-36 h at the temperature of 60-80 ℃, and the freeze drying is drying for 36-48 h at the temperature of-30-40 ℃.
The other purpose of the invention is realized by the following technical scheme:
the invention provides a method for doping CaTi by utilizing the velvet interweaving spheroidal carbon and nitrogen2O4(OH)2The product prepared by the preparation method of the porous nano material has a shape structure of a porous network structure formed by uniformly distributing micropores and mesopores; the micropores and the mesopores are formed by mutually connecting, staggering and uniformly distributing nanosheets, wherein the aperture of each micropore is 3-5 nm, and the aperture of each mesopore is 8-30 nm; the length of the nanosheet is 200-500 nm, the width of the nanosheet is 30-200 nm, the thickness of the nanosheet is less than 30nm, and the nanosheet is in a long-edge micro-roll shape.
The invention provides a method for doping CaTi by utilizing the velvet interweaving spheroidal carbon and nitrogen2O4(OH)2The product prepared by the preparation method of the porous nano material is applied to an electrode material of a super capacitor.
The invention has the following beneficial effects:
(1) to maintain feather structural integrity while maintaining CaTi2O4(OH)2The precursor is not destroyed in the solvent reaction process, the invention firstly prepares CaTi2O4(OH)2Precursor solution is prepared through protecting precursor in micro reactor formed by mixing proper water and alcohol, adding feather without being carbonized, carbonizing feather to produce great amount of functional groups by changing pH value in solvent heating process, and strengthening adsorption force to obtain CaTi2O4(OH)2The precursor solution was fully attached to the feather. The invention well keeps the microstructure of the feather, not only improves the pore structure distribution, but also has larger specific surface area; simultaneously overcomes the defect that the feather is treated by adopting a complex C-type process and then compounded with other materials in the current researchThe synthesis process has the advantages of complexity, simple operation, low cost, less energy consumption and no toxic substances.
(2) The invention relates to a velvet interweaving spheroidal carbon-nitrogen-doped CaTi2O4(OH)2The porous nano material has good dispersibility, presents a long-side micro-rolling nano sheet structure, and leads the down feather interweaving spheroidal carbon nitrogen doped CaTi2O4(OH)2Porous nano electrode material purer CaTi2O4(OH)2The porous nano electrode material has more excellent electrochemical performance, good rate performance and good charge-discharge efficiency.
Drawings
The invention will now be described in further detail with reference to the following examples and the accompanying drawings:
FIG. 1 shows a down feather interwoven spheroidal carbon-nitrogen doped CaTi prepared by the method of the embodiment of the invention2O4(OH)2Scanning electron microscope pictures of the porous nano-materials (a: 20000, b: 100000);
FIG. 2 shows a down feather interwoven spheroidal carbon-nitrogen doped CaTi prepared by the method of the embodiment of the invention2O4(OH)2An X-ray diffraction pattern of the porous nanomaterial;
FIG. 3 shows a down feather interwoven spheroidal carbon-nitrogen doped CaTi prepared by the method of the embodiment of the invention2O4(OH)2EDS energy spectrum of the porous nano material;
FIG. 4a shows a down feather interwoven spheroidal carbon-nitrogen doped CaTi prepared by the method of the embodiment of the invention2O4(OH)2Pore size distribution map of porous nanomaterial;
FIG. 4b shows the down-feather interlaced sphere-like carbon-nitrogen doped CaTi prepared by the embodiment of the present invention2O4(OH)2The specific surface area BET of the porous nanomaterial;
FIG. 5 shows a down feather interwoven spheroidal carbon-nitrogen doped CaTi prepared by the method of the embodiment of the invention2O4(OH)2Porous nano electrode material and pure CaTi2O4(OH)2A schematic diagram of cyclic voltammograms of the electrode material at a rate of 10 mV/s;
FIG. 6a is an embodiment of the present inventionThe obtained down feather interweaving spheroidal carbon and nitrogen doped CaTi2O4(OH)2Porous nano electrode material and pure CaTi2O4(OH)2The electrode material is 10mA/cm2A schematic diagram of a comparative constant current charge-discharge curve at speed;
FIG. 6b is pure CaTi2O4(OH)2A schematic diagram of cyclic voltammograms of the electrode material at a rate of 10 mV/s;
FIG. 7 shows a down feather interwoven spheroidal carbon and nitrogen doped CaTi prepared by the method of the embodiment of the invention2O4(OH)2A schematic diagram of cyclic voltammetry curve of the porous nano-electrode material;
FIG. 8 shows a down feather interwoven spheroidal carbon-nitrogen doped CaTi prepared by the method of the embodiment of the invention2O4(OH)2Constant current charge and discharge curve of the porous nano electrode material.
Detailed Description
The first embodiment is as follows:
this example shows a down-feather interlaced spheroidal carbon-nitrogen doped CaTi2O4(OH)2The preparation method of the porous nano material comprises the following steps:
(1) soaking the feathers in a chlorine dioxide solution for 24 hours for sterilization, then washing the sterilized feathers with distilled water for 5 times, soaking the feathers in an ethanol solution for 1 day for secondary sterilization and carrying out ultrasonic oscillation for 30min, then washing the feathers with distilled water for 5 times, and naturally drying the feathers in a ventilated place to obtain pretreated feathers; wherein, the weight ratio of the feather to the chlorine dioxide solution to the distilled water to the ethanol is 1: 500: 5;
(2) dissolving tetra-n-butyl titanate in ethanol according to a molar ratio of 1: 7.5 to ethanol, stirring and mixing for 5min to obtain a solution A;
(3) dissolving anhydrous calcium chloride in distilled water according to the molar ratio of the calcium chloride to the distilled water to the ethanol of 10: 500: 15, adding the ethanol, stirring and mixing for 7min to obtain a solution B;
(4) slowly dropping the solution A into the solution B according to the mol ratio of calcium chloride to tetra-n-butyl titanate of 1: 1, stirring and mixing for 10min, and gradually dropping hydrogenAdjusting the pH value of the sodium oxide solution to 8, continuously stirring and mixing for 15min for the second time to obtain CaTi2O4(OH)2A precursor;
(5) according to the mass ratio of CaTi2O4(OH)2Stirring and mixing the precursor and the pretreated feather for 5min, putting the mixture into a hydrothermal reaction kettle, keeping the temperature at 180 ℃ for 24h, washing the reaction product with distilled water for 7 times, then washing the reaction product with ethanol for 5 times, filtering the reaction product, and freeze-drying the reaction product at-30 ℃ for 48h to obtain the down-feather interwoven spheroidal carbon-nitrogen-doped CaTi2O4(OH)2A porous nanomaterial.
Example two:
this example shows a down-feather interlaced spheroidal carbon-nitrogen doped CaTi2O4(OH)2The preparation method of the porous nano material comprises the following steps:
(1) soaking the feathers in a chlorine dioxide solution for 20 hours for sterilization, then washing the sterilized feathers with distilled water for 6 times, soaking the feathers in an ethanol solution for 2 days for secondary sterilization and carrying out ultrasonic oscillation for 30min, then washing the feathers with distilled water for 6 times, and naturally drying the feathers in a ventilated place to obtain pretreated feathers; wherein, the weight ratio of the feather to the chlorine dioxide solution to the distilled water to the ethanol is 5: 2: 1000: 20;
(2) dissolving tetra-n-butyl titanate in ethanol according to a molar ratio of tetra-n-butyl titanate to ethanol of 1: 8, stirring and mixing for 8min to obtain a solution A;
(3) dissolving anhydrous calcium chloride in distilled water according to the molar ratio of 5: 300: 10, adding ethanol, stirring and mixing for 5min to obtain a solution B;
(4) slowly dropping the solution A into the solution B according to the mol ratio of calcium chloride to tetra-n-butyl titanate of 1: 1.2, stirring and mixing for the first time for 15min, gradually dropping sodium hydroxide solution to adjust the pH value to 7.5, continuously stirring and mixing for the second time for 25min to obtain CaTi2O4(OH)2A precursor;
(5) according to the mass ratio of CaTi2O4(OH)2Mixing the precursor and the pretreated feather at a ratio of 1: 0.4 under stirring for 10minPlacing into a hydrothermal reaction kettle, keeping the temperature at 160 ℃ for 18h, washing the reaction product with distilled water for 7 times, then washing with ethanol for 5 times, filtering, and freeze-drying at-35 ℃ for 42h to obtain the down-feather interweaving spheroidal carbon and nitrogen doped CaTi2O4(OH)2A porous nanomaterial.
Example three:
this example shows a down-feather interlaced spheroidal carbon-nitrogen doped CaTi2O4(OH)2The preparation method of the porous nano material comprises the following steps:
(1) soaking the feathers in a chlorine dioxide solution for 18h for sterilization, then washing the sterilized feathers with distilled water for 7 times, soaking the feathers in an ethanol solution for 2 days for secondary sterilization and carrying out ultrasonic oscillation for 30min, then washing the feathers with distilled water for 7 times, and naturally drying the feathers in a ventilated place to obtain pretreated feathers; wherein, the weight ratio of the feather to the chlorine dioxide solution to the distilled water to the ethanol is 10: 3: 1500: 35;
(2) dissolving tetra-n-butyl titanate in ethanol according to a molar ratio of 1: 8.5 to ethanol, stirring and mixing for 10min to obtain a solution A;
(3) dissolving anhydrous calcium chloride in distilled water according to the molar ratio of the calcium chloride to the distilled water to the ethanol of 15: 400: 20, adding the ethanol, stirring and mixing for 8min to obtain a solution B;
(4) slowly dropping the solution A into the solution B according to the mol ratio of calcium chloride to tetra-n-butyl titanate of 1: 1.4, stirring and mixing for one time for 20min, gradually dropping sodium hydroxide solution to adjust the pH value to 8.5, continuously stirring and mixing for another time for 35min to obtain CaTi2O4(OH)2A precursor;
(5) according to the mass ratio of CaTi2O4(OH)2Stirring and mixing the precursor and the pretreated feather for 15min, putting the mixture into a hydrothermal reaction kettle, preserving heat for 30h at the hydrothermal temperature of 200 ℃, washing the reaction product with distilled water for 7 times, then washing the reaction product with ethanol for 5 times, filtering the reaction product, and freeze-drying the reaction product for 36h at the temperature of-40 ℃ to obtain the down-feather interwoven spheroidal carbon and nitrogen doped CaTi2O4(OH)2A porous nanomaterial.
Example four:
this example shows a down-feather interlaced spheroidal carbon-nitrogen doped CaTi2O4(OH)2The preparation method of the porous nano material comprises the following steps:
(1) soaking the feathers in a chlorine dioxide solution for 22h for disinfection, then washing the disinfected feathers with distilled water for 8 times, soaking the feathers in an ethanol solution for 2 days for secondary disinfection and carrying out ultrasonic oscillation for 30min, then washing the feathers with distilled water for 8 times, and naturally drying the feathers in a ventilated place to obtain pretreated feathers; wherein, the weight ratio of the feather to the chlorine dioxide solution to the distilled water to the ethanol is 15: 4: 2000: 50;
(2) dissolving tetra-n-butyl titanate in ethanol according to a molar ratio of tetra-n-butyl titanate to ethanol of 1: 8, stirring and mixing for 10min to obtain a solution A;
(3) dissolving anhydrous calcium chloride in distilled water according to the molar ratio of 20: 450: 15, adding ethanol, stirring and mixing for 9min to obtain solution B;
(4) slowly dropping the solution A into the solution B according to the mol ratio of calcium chloride to tetra-n-butyl titanate of 1: 1.6, stirring and mixing for the first time for 15min, gradually dropping sodium hydroxide solution to adjust the pH value to 8, continuously stirring and mixing for the second time for 30min to obtain CaTi2O4(OH)2A precursor;
(5) according to the mass ratio of CaTi2O4(OH)2Stirring and mixing the precursor and the pretreated feather for 20min, putting the mixture into a hydrothermal reaction kettle, keeping the temperature at 180 ℃ for 24h, washing the reaction product with distilled water for 7 times, then washing the reaction product with ethanol for 5 times, filtering the reaction product, and drying the reaction product in vacuum at 60 ℃ for 36h to obtain the down-feather interwoven spheroidal carbon and nitrogen doped CaTi2O4(OH)2A porous nanomaterial.
Example five:
this example shows a down-feather interlaced spheroidal carbon-nitrogen doped CaTi2O4(OH)2The preparation method of the porous nano material comprises the following steps:
(1) soaking the feathers in a chlorine dioxide solution for 24 hours for sterilization, then washing the sterilized feathers with distilled water for 10 times, soaking the feathers in an ethanol solution for 2 days for secondary sterilization and carrying out ultrasonic oscillation for 30min, then washing the feathers with distilled water for 10 times, and naturally drying the feathers in a ventilated place to obtain pretreated feathers; wherein, the weight ratio of the feather to the chlorine dioxide solution to the distilled water to the ethanol is 20: 5: 2000: 50;
(2) dissolving tetra-n-butyl titanate in ethanol according to a molar ratio of tetra-n-butyl titanate to ethanol of 1: 8, stirring and mixing for 7min to obtain a solution A;
(3) dissolving anhydrous calcium chloride in distilled water according to the molar ratio of the calcium chloride to the distilled water to the ethanol of 25: 350: 15, adding the ethanol, stirring and mixing for 10min to obtain a solution B;
(4) slowly dropping the solution A into the solution B according to the mol ratio of calcium chloride to tetra-n-butyl titanate of 1: 1.8, stirring and mixing for the first time for 15min, gradually dropping sodium hydroxide solution to adjust the pH value to 8, continuously stirring and mixing for the second time for 20min to obtain CaTi2O4(OH)2A precursor;
(5) according to the mass ratio of CaTi2O4(OH)2Stirring and mixing the precursor and the pretreated feather for 20min, putting the mixture into a hydrothermal reaction kettle, keeping the temperature at 160 ℃ for 24h, washing the reaction product with distilled water for 7 times, then washing the reaction product with ethanol for 5 times, filtering the reaction product, and drying the reaction product in vacuum at 70 ℃ for 30h to obtain the down-feather interwoven spheroidal carbon and nitrogen doped CaTi2O4(OH)2A porous nanomaterial.
Example six:
this example shows a down-feather interlaced spheroidal carbon-nitrogen doped CaTi2O4(OH)2The preparation method of the porous nano material comprises the following steps:
(1) soaking the feathers in a chlorine dioxide solution for 18h for sterilization, then washing the sterilized feathers with distilled water for 8 times, soaking the feathers in an ethanol solution for 1 day for secondary sterilization and carrying out ultrasonic oscillation for 30min, then washing the feathers with distilled water for 10 times, and naturally drying the feathers in a ventilated place to obtain pretreated feathers; wherein, the weight ratio of the feather to the chlorine dioxide solution to the distilled water to the ethanol is 10: 5: 1500: 35;
(2) dissolving tetra-n-butyl titanate in ethanol according to a molar ratio of tetra-n-butyl titanate to ethanol of 1: 8, stirring and mixing for 6min to obtain a solution A;
(3) dissolving anhydrous calcium chloride in distilled water according to the molar ratio of the calcium chloride to the distilled water to the ethanol of 10: 450: 15, adding the ethanol, stirring and mixing for 10min to obtain a solution B;
(4) slowly dropping the solution A into the solution B according to the molar ratio of calcium chloride to tetra-n-butyl titanate of 1: 2, stirring and mixing for 20min for the first time, gradually dropping sodium hydroxide solution to adjust the pH value to 8, continuously stirring and mixing for 10min for the second time to obtain CaTi2O4(OH)2A precursor;
(5) according to the mass ratio of CaTi2O4(OH)2Stirring and mixing the precursor and the pretreated feather for 10min, putting the mixture into a hydrothermal reaction kettle, keeping the temperature at 180 ℃ for 24h, washing the reaction product with distilled water for 7 times, then washing the reaction product with ethanol for 5 times, filtering the reaction product, and drying the reaction product in vacuum at 80 ℃ for 24h to obtain the down-feather interwoven spheroidal carbon and nitrogen doped CaTi2O4(OH)2A porous nanomaterial.
As shown in FIG. 1, the velvet interlaced spherical carbon-nitrogen-doped CaTi prepared by the embodiment of the invention2O4(OH)2The porous nano material is uniformly distributed like a sphere under a 2 ten thousand times scanning electron microscope (see figure 1a), and is formed into a porous structure with micropores (the aperture is 3-5 nm) and mesopores (the aperture is 8-30 nm) by mutually connecting and distributing nano sheets with long edge micro-roll, the length is 200-500 nm and the width is 30-200 nm under a 10 ten thousand times scanning electron microscope (see figure 1b and figure 4 a).
As shown in FIG. 2, the velvet interlaced spherical carbon-nitrogen-doped CaTi prepared by the embodiment of the invention2O4(OH)2The characteristic diffraction peaks of the porous nanomaterial are partially uniform and enhanced, with the 2 θ angle shifted to the right by about 0.5 °.
As shown in FIG. 3, the velvet interlaced spherical carbon-nitrogen-doped CaTi prepared by the embodiment of the invention2O4(OH)2Porous nanoparticlesMaterials other than CaTi2O4(OH)2The elements Ca, Ti and O in (1) further contain C, P, S, N, Pt, which is described in CaTi2O4(OH)2A small amount of C, N is doped in the component (A), and a small amount of P, S is also doped in the component (B), so that the C, N atomic radius is small, the crystal lattice distortion occurs, and the XRD diffraction peak shifts to the right, wherein Pt is caused by spraying platinum.
As shown in FIG. 4a, the velvet interlaced spherical carbon-nitrogen-doped CaTi prepared by the embodiment of the invention2O4(OH)2A porous nanomaterial having an average pore size of 12.9248 nm; BET specific surface area of 510.9175m as shown in FIG. 4b2/g。
As shown in FIG. 5, the velvet interlaced spherical carbon-nitrogen-doped CaTi prepared by the embodiment of the invention2O4(OH)2The area surrounded by the cyclic voltammetry curve of the porous nano material is larger, and the oxidation-reduction peak is symmetrical and obvious, which shows that the specific capacitance is larger, the storage charge capacity is more and the electrochemical performance is excellent under the same scanning speed.
Calculated according to formula 1, the velvet interweaved spheroidal carbon-nitrogen-doped CaTi prepared by the embodiment of the invention2O4(OH)2Porous nanomaterial and pure CaTi2O4(OH)2Electrode material at an operating current density of 10mA/cm2The specific capacitances of (A) are 1513.1F g-1、227.8F*g-1。
As can be seen from FIG. 6a, the constant current charging and discharging curves before and after doping of the sample are similar in characteristics, and both have a charging and discharging platform in the range of 0.3V to 0.35V and 10mA/cm2When the specific capacitance is pure CaTi2O4(OH)2The specific capacitance of the electrode material is 6.6 times that of the electrode material, which shows that the electrode material has good rate performance. FIG. 6b is an enlarged graph of FIG. 6a, showing that the symmetry curve is similar to the curve after doping, and further illustrating that the CaTi is unchanged after doping2O4(OH)2Crystal structure, which is consistent with XRD results.
As shown in FIG. 7, the down-feather interlaced sphere-like carbon-nitrogen-doped CaTi prepared by the embodiment of the invention2O4(OH)2The porous nano material has good oxidation-reduction peak symmetry, the peak height is increased along with the increase of the scanning speed, and the oxidation-reduction peaks respectively move towards the positive direction and the negative direction, which shows that the velvet interweaved spheroidal carbon nitrogen is doped with CaTi2O4(OH)2The porous nano electrode material has quick current response and good rate performance, and can meet the requirement of quick charge and discharge of a super capacitor.
As shown in FIG. 8, the down-feather interlaced sphere-like carbon-nitrogen-doped CaTi prepared by the embodiment of the invention2O4(OH)2The CP curve of the porous nano material is different from that of a standard isosceles triangle, and the CP curve may be interwoven with the down feather to form the spherical carbon and nitrogen doped CaTi2O4(OH)2The porous nano electrode material has related Faraday pseudocapacitance effect. The velvet interweaved spheroidal carbon-nitrogen-doped CaTi can be obtained by calculation according to the formula 12O4(OH)2The working current density of the porous nano electrode material is 10mA/cm2、20mA/cm2、50mA/cm2、100mA/cm2、200mA/cm2The specific capacitances are 1513.1F g-1、1271.3F*g-1、984.4F*g-1、787.5F*g-1、562.5F*g-1. Along with the increase of current density, the velvet interweaved spheroidal carbon-nitrogen-doped CaTi2O4(OH)2The reason why the specific capacitance of the porous nano-electrode material gradually decreases is that the rate of the redox reaction of the electrode active material and the rate of charge diffusion are lower than the charge-discharge rate of the capacitor. As can also be seen from FIG. 6, the down-feather interlaced spheroidal carbon-nitrogen-doped CaTi2O4(OH)2The porous nano electrode material has uniform CP curve shape, and shows excellent rate capability and charge-discharge performance of the electrode material.
Claims (10)
1. Velvet-interwoven spheroidal carbon-nitrogen-doped CaTi2O4(OH)2The preparation method of the porous nano material is characterized by comprising the following steps:
(1) disinfecting, washing and drying the feathers to obtain pretreated feathers;
(2) dissolving tetra-n-butyl titanate in ethanol according to a molar ratio of 1: 7.5-8.5, and stirring and mixing to obtain a solution A;
(3) dissolving anhydrous calcium chloride into distilled water according to the molar ratio of 5-25: 300-500: 10-20 of calcium chloride to distilled water to ethanol, adding ethanol, and stirring and mixing to obtain a solution B;
(4) adding the solution A into the solution B according to the molar ratio of calcium chloride to tetra-n-butyl titanate of 1: 1-2, stirring and mixing for the first time, adding an alkaline solution to adjust the pH value to 7.5-8.5, and continuously stirring and mixing for the second time to obtain CaTi2O4(OH)2A precursor;
(5) according to the mass ratio of CaTi2O4(OH)2Stirring and mixing the precursor and the pretreated feather at the ratio of 1: 0.1-1.2, putting the mixture into a hydrothermal reaction kettle, preserving the heat for 18-30 hours at the hydrothermal temperature of 160-200 ℃, washing, filtering and drying a reaction product to obtain the feather interwoven spheroidal carbon and nitrogen doped CaTi2O4(OH)2A porous nanomaterial.
2. The velvet interwoven spheroidal carbon nitrogen-doped CaTi as claimed in claim 12O4(OH)2The preparation method of the porous nano material is characterized by comprising the following steps: in the step (1), the feathers are soaked in a chlorine dioxide solution for 18-24 hours for disinfection, then the disinfected feathers are washed with distilled water for 5-10 times, then soaked in an ethanol solution for 1-2 days for secondary disinfection and subjected to ultrasonic oscillation for 30min, then washed with distilled water for 5-10 times, and the feathers are placed in a ventilated place for natural drying to obtain the pretreated feathers.
3. The velvet interwoven spheroidal carbon nitrogen-doped CaTi as claimed in claim 22O4(OH)2The preparation method of the porous nano material is characterized by comprising the following steps: according toThe weight ratio of the feather to the chlorine dioxide solution to the distilled water to the ethanol is 1-20: 1-5: 500-2000: 5-50.
4. The velvet interwoven spheroidal carbon nitrogen-doped CaTi as claimed in claim 12O4(OH)2The preparation method of the porous nano material is characterized by comprising the following steps: the feather is bird feather.
5. The velvet interwoven spheroidal carbon nitrogen-doped CaTi as claimed in claim 12O4(OH)2The preparation method of the porous nano material is characterized by comprising the following steps: the alkaline solution is one or the combination of sodium hydroxide solution, ammonia water and potassium hydroxide solution.
6. The velvet interwoven spheroidal carbon nitrogen-doped CaTi as claimed in claim 12O4(OH)2The preparation method of the porous nano material is characterized by comprising the following steps: the stirring and mixing time of the step (2) is 5-10 min; the stirring and mixing time of the step (3) is 5-10 min; the primary stirring and mixing time of the step (4) is 10-20 min, and the secondary stirring and mixing time is 15-35 min; and (5) stirring and mixing for 5-20 min.
7. The velvet interwoven spheroidal carbon nitrogen-doped CaTi as claimed in claim 12O4(OH)2The preparation method of the porous nano material is characterized by comprising the following steps: the drying in the step (5) is vacuum drying or freeze drying, wherein the vacuum drying is drying for 24-36 h at the temperature of 60-80 ℃, and the freeze drying is drying for 36-48 h at the temperature of-30-40 ℃.
8. Doping CaTi with the feather-interweaving spheroidal carbon-nitrogen according to any of claims 1 to 72O4(OH)2The product is prepared by the preparation method of the porous nano material.
9. The method of claim 8, wherein the blended carbon and nitrogen CaTi is spherical carbon and nitrogen2O4(OH)2The product prepared by the preparation method of the porous nano material is characterized in that: the morphology structure is a porous network structure formed by uniformly distributing micropores and mesopores; the micropores and the mesopores are formed by mutually connecting and distributing nanosheets in a staggered manner, the aperture of each micropore is 3-5 nm, and the aperture of each mesopore is 8-30 nm; the length of the nanosheet is 200-500 nm, the width of the nanosheet is 30-200 nm, the thickness of the nanosheet is less than 30nm, and the nanosheet is in a long-edge micro-roll shape.
10. Doping CaTi with the feather-interweaving spheroidal carbon-nitrogen according to any of claims 1 to 72O4(OH)2The application of the product prepared by the preparation method of the porous nano material is characterized in that: the product is used for an electrode material of a super capacitor.
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