CN113838676B - Down feather interwoven spheroidal carbon-nitrogen-doped CaTi 2 O 4 (OH) 2 Preparation method of porous nano material - Google Patents
Down feather interwoven spheroidal carbon-nitrogen-doped CaTi 2 O 4 (OH) 2 Preparation method of porous nano material Download PDFInfo
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- 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
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- 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
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a down feather interwoven spheroidal carbon and nitrogen doped CaTi 2 O 4 (OH) 2 The preparation method of the porous nano material comprises the steps of firstly preparing CaTi 2 O 4 (OH) 2 The precursor solution is combined with non-carbonized feathers, and the porous nanomaterial with excellent electrochemical performance and serving as the electrode material of the supercapacitor is obtained by adopting solvothermal process with simple operation and low cost. In addition, the velvet interweaved spheroidal carbon-nitrogen-doped CaTi is also disclosed 2 O 4 (OH) 2 The 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 CaTi 2 O 4 (OH) 2 A 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 CaTi 2 O 4 (OH) 2 The nano structure has better electrochemical performance, meets the mechanism of Faraday pseudo-capacitance charge storage, has simple preparation process and low cost, but is pure CaTi 2 O 4 (OH) 2 The nano sheet has poor conductivity, and the charging and discharging curves are not symmetrical enough, so the cycling stability is poor. For this purpose, the specific surface area of 600m was prepared 2 CaTi of/g 2 O 4 (OH) 2 The honeycomb-shaped powder has larger specific surface area, but has larger pore size distribution (80-165 nm), and has poorer electrochemical performance. 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 CaTi 2 O 4 (OH) 2 The 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, and the operation is simple and the cost is low. Another object of the present invention is to provideDoping CaTi with the velvet interweaving spheroidal carbon and nitrogen 2 O 4 (OH) 2 The 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 interwoven spheroidal carbon and nitrogen doped CaTi 2 O 4 (OH) 2 The 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 the molar ratio of tetra-n-butyl titanate to ethanol = 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 mol ratio of the calcium chloride to the distilled water to the ethanol = 5-25: 300-500: 10-20, then adding the ethanol, stirring and mixing to obtain a solution B;
(4) According to the mol ratio of calcium chloride to tetra-n-butyl titanate = 1: 1-2, adding the solution A into the solution B, 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 CaTi 2 O 4 (OH) 2 A precursor;
(5) According to the mass ratio of CaTi 2 O 4 (OH) 2 The precursor and the pretreated feather are = 1: 0.1-1.2, stirred and mixed, then put into a hydrothermal reaction kettle, kept at the hydrothermal temperature of 160-200 ℃ for 18-30 h, and the reaction product is washed, filtered and dried to obtain the down-feather interweaving spheroidal carbon and nitrogen doped CaTi 2 O 4 (OH) 2 A 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 taken as a natural product, naturally inherits C, N, P and S elements and has remarkable fine keratin lengthThe silk, under proper treatment, can produce a highly active carbon-nitrogen doped porous structure. 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 method 2 O 4 (OH) 2 Thereby preparing the electrode material with adjustable pore size distribution, stable electrochemical performance, high specific capacitance and excellent rate performance.
Further, in the step (1) of the preparation method, the feather is soaked in 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 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 naturally dried in a ventilated place to obtain the pretreated feather. Wherein, the feather, the chlorine dioxide solution, the distilled water and the ethanol are mixed according to the weight ratio of 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 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; the stirring and mixing time of the step (5) is 5-20 min. The drying in the step (5) is vacuum drying or freeze drying, wherein the vacuum drying is drying for 24 to 36 hours at the temperature of between 60 and 80 ℃, and the freeze drying is drying for 36 to 48 hours at the temperature of between 30 ℃ below zero and 40 ℃ below zero.
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 nitrogen 2 O 4 (OH) 2 The 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 connected with each other by nano sheets, staggered and uniformly distributedThe aperture of the micropores is 3-5 nm, and the aperture of the mesopores is 8-30 nm; the length of the nano sheet is 200-500 nm, the width of the nano sheet is 30-200 nm, the thickness of the nano sheet is less than 30nm, and the long side of the nano sheet is micro-rolled.
The invention provides a method for doping CaTi by utilizing the velvet interweaving spheroidal carbon and nitrogen 2 O 4 (OH) 2 The 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 CaTi 2 O 4 (OH) 2 The precursor is not destroyed in the solvent reaction process, the invention firstly prepares CaTi 2 O 4 (OH) 2 Precursor 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 CaTi 2 O 4 (OH) 2 The precursor solution was fully attached to the feathers. The invention well keeps the microstructure of the feather, not only improves the pore structure distribution, but also has larger specific surface area; meanwhile, the method overcomes the complexity of processes of treating the feathers by adopting a complex C-process and then compounding the feathers with other materials in the prior research, and has the advantages of simple operation, low cost, less energy consumption and no toxic substance generation.
(2) The invention relates to a velvet interweaving spheroidal carbon-nitrogen-doped CaTi 2 O 4 (OH) 2 The 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 CaTi 2 O 4 (OH) 2 Porous nano electrode material purer CaTi 2 O 4 (OH) 2 The 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 embodiment of the invention 2 O 4 (OH) 2 Scanning electron microscopy of porous nanomaterials (a: 20000, b;
FIG. 2 shows a down feather interwoven spheroidal carbon nitrogen doped CaTi prepared by the embodiment of the invention 2 O 4 (OH) 2 An 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 invention 2 O 4 (OH) 2 EDS energy spectrum of the porous nano material;
FIG. 4a shows a down feather interwoven spheroidal carbon nitrogen doped CaTi prepared by the embodiment of the invention 2 O 4 (OH) 2 Pore 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 invention 2 O 4 (OH) 2 The 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 invention 2 O 4 (OH) 2 Porous nano electrode material and pure CaTi 2 O 4 (OH) 2 A schematic diagram of cyclic voltammograms of the electrode material at a rate of 10 mV/s;
FIG. 6a shows a down feather interwoven spheroidal carbon nitrogen doped CaTi prepared by the embodiment of the invention 2 O 4 (OH) 2 Porous nano electrode material and pure CaTi 2 O 4 (OH) 2 The electrode material is 10mA/cm 2 A schematic diagram of a comparative constant current charge-discharge curve at speed;
FIG. 6b is pure CaTi 2 O 4 (OH) 2 A 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 nitrogen doped CaTi prepared by the embodiment of the invention 2 O 4 (OH) 2 A 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 invention 2 O 4 (OH) 2 Porous nanoelectricsConstant current charge and discharge curve of the electrode material.
Detailed Description
The first embodiment is as follows:
this example shows a down feather interwoven spheroidal carbon nitrogen doped CaTi 2 O 4 (OH) 2 The 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 feather, the chlorine dioxide solution, the distilled water and the ethanol are mixed according to the weight ratio of 1: 500: 5;
(2) Dissolving tetra-n-butyl titanate in ethanol according to a molar ratio of tetra-n-butyl titanate to ethanol = 1: 7.5, stirring and mixing for 5min to obtain a solution A;
(3) Dissolving anhydrous calcium chloride in distilled water according to the molar ratio of calcium chloride to distilled water to ethanol = 10: 500: 15, adding 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 = 1: 1, stirring and mixing for the first time for 10min, gradually dropping sodium hydroxide solution to adjust the pH value to 8, continuously stirring and mixing for the second time for 15min to obtain CaTi 2 O 4 (OH) 2 A precursor;
(5) According to the mass ratio of CaTi 2 O 4 (OH) 2 Stirring 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 and nitrogen doped CaTi 2 O 4 (OH) 2 A porous nanomaterial.
Example two:
this example shows a down-feather interlaced spheroidal carbon-nitrogen doped CaTi 2 O 4 (OH) 2 Preparation of porous nano materialThe preparation method 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 feather, the chlorine dioxide solution, the distilled water and the ethanol are mixed according to the weight ratio of 5: 2: 1000: 20;
(2) Dissolving tetra-n-butyl titanate in ethanol according to a molar ratio of tetra-n-butyl titanate to ethanol = 1: 8, stirring and mixing for 8min to obtain a solution A;
(3) Dissolving anhydrous calcium chloride in distilled water according to the mol ratio of the calcium chloride to the distilled water to the ethanol = 5: 300: 10, then adding the 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 = 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, and continuously stirring and mixing for the second time for 25min to obtain CaTi 2 O 4 (OH) 2 A precursor;
(5) According to the mass ratio of CaTi 2 O 4 (OH) 2 Precursor and pretreated feather = 1: 0.4, stirred and mixed for 10min, then placed into a hydrothermal reaction kettle, heat-preserved for 18h at the hydrothermal temperature of 160 ℃, reaction products are washed by distilled water for 7 times and then by ethanol for 5 times, and freeze-dried for 42h at the temperature of-35 ℃ after filtration to obtain the down feather interwoven spheroidal carbon and nitrogen doped CaTi 2 O 4 (OH) 2 A porous nanomaterial.
Example three:
this example shows a down-feather interlaced spheroidal carbon-nitrogen doped CaTi 2 O 4 (OH) 2 The 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 feather, the chlorine dioxide solution, the distilled water and the ethanol are mixed according to the weight ratio of 10: 3: 1500: 35;
(2) Dissolving tetra-n-butyl titanate in ethanol according to a molar ratio of tetra-n-butyl titanate to ethanol = 1: 8.5, and stirring and mixing for 10min to obtain a solution A;
(3) Dissolving anhydrous calcium chloride in distilled water according to the molar ratio of calcium chloride to distilled water to ethanol = 15: 400: 20, adding ethanol, stirring and mixing for 8min to obtain a solution B;
(4) Slowly dripping the solution A into the solution B according to the mol ratio of calcium chloride to tetra-n-butyl titanate = 1: 1.4, stirring and mixing for the first time for 20min, gradually dripping sodium hydroxide solution to adjust the pH value to 8.5, and continuously stirring and mixing for the second time for 35min to obtain CaTi 2 O 4 (OH) 2 A precursor;
(5) According to the mass ratio of CaTi 2 O 4 (OH) 2 Precursor and pretreated feather = 1: 0.8, stirred and mixed for 15min, then placed into a hydrothermal reaction kettle, heat-preserved for 30h at the hydrothermal temperature of 200 ℃, reaction products are washed by distilled water for 7 times and then by ethanol for 5 times, and freeze-dried for 36h at the temperature of-40 ℃ after filtration to obtain the down feather interwoven spheroidal carbon and nitrogen doped CaTi 2 O 4 (OH) 2 A porous nanomaterial.
Example four:
this example shows a down-feather interlaced spheroidal carbon-nitrogen doped CaTi 2 O 4 (OH) 2 The 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 feather, the chlorine dioxide solution, the distilled water and the ethanol are mixed according to the weight ratio of 15: 4: 2000: 50;
(2) Dissolving tetra-n-butyl titanate in ethanol according to the molar ratio of tetra-n-butyl titanate to ethanol = 1: 8, stirring and mixing for 10min to obtain a solution A;
(3) Dissolving anhydrous calcium chloride in distilled water according to the mol ratio of the calcium chloride to the distilled water to the ethanol = 20: 450: 15, adding the ethanol, stirring and mixing for 9min 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 = 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 CaTi 2 O 4 (OH) 2 A precursor;
(5) According to the mass ratio of CaTi 2 O 4 (OH) 2 Stirring 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 CaTi 2 O 4 (OH) 2 A porous nanomaterial.
Example five:
this example shows a down feather interwoven spheroidal carbon nitrogen doped CaTi 2 O 4 (OH) 2 The preparation method of the porous nano material comprises the following steps:
(1) Soaking the feathers in a chlorine dioxide solution for 24 hours for disinfection, then washing the disinfected feathers with distilled water for 10 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 10 times, and naturally drying the feathers at a ventilated place to obtain pretreated feathers; wherein, the feather, the chlorine dioxide solution, the distilled water and the ethanol are mixed according to the weight ratio of 20: 5: 2000: 50;
(2) Dissolving tetra-n-butyl titanate in ethanol according to a molar ratio of tetra-n-butyl titanate to ethanol = 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 calcium chloride to distilled water to ethanol = 25: 350: 15, adding ethanol, stirring and mixing for 10min to obtain a solution B;
(4) According to the mole ratio of chlorinationCalcium and tetra-n-butyl titanate = 1: 1.8, the solution A is slowly dripped into the solution B to be stirred and mixed for 15min for the first time, then sodium hydroxide solution is gradually dripped to adjust the pH value to 8, and the secondary stirring and mixing are continued for 20min to obtain CaTi 2 O 4 (OH) 2 A precursor;
(5) According to the mass ratio of CaTi 2 O 4 (OH) 2 Precursor and pretreated feather = 1: 0.1, stirred and mixed for 20min, then placed into a hydrothermal reaction kettle, kept at the hydrothermal temperature of 160 ℃ for 24h, washed by distilled water for 7 times, then washed by ethanol for 5 times, filtered and dried in vacuum at the temperature of 70 ℃ for 30h to obtain the down-feather interwoven spheroidal carbon and nitrogen doped CaTi 2 O 4 (OH) 2 A porous nanomaterial.
Example six:
this example shows a down feather interwoven spheroidal carbon nitrogen doped CaTi 2 O 4 (OH) 2 The preparation method of the porous nano material comprises the following steps:
(1) Soaking the feathers in a chlorine dioxide solution for 18h for disinfection, then washing the disinfected feathers with distilled water for 8 times, soaking the feathers in an ethanol solution for 1 day for secondary disinfection and carrying out ultrasonic oscillation for 30min, then washing the feathers with distilled water for 10 times, and naturally drying the feathers at a ventilated place to obtain pretreated feathers; wherein, the feather, the chlorine dioxide solution, the distilled water and the ethanol are mixed according to the weight ratio of 10: 5: 1500: 35;
(2) Dissolving tetra-n-butyl titanate in ethanol according to the molar ratio of tetra-n-butyl titanate to ethanol = 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 calcium chloride to distilled water to ethanol = 10: 450: 15, adding 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 = 1: 2, stirring and mixing for the first time for 20min, gradually dropping sodium hydroxide solution to adjust the pH value to 8, continuously stirring and mixing for the second time for 10min to obtain CaTi 2 O 4 (OH) 2 A precursor;
(5) According to the mass ratio of CaTi 2 O 4 (OH) 2 Stirring 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 CaTi 2 O 4 (OH) 2 A porous nanomaterial.
As shown in FIG. 1, the velvet interlaced spherical carbon-nitrogen-doped CaTi prepared by the embodiment of the invention 2 O 4 (OH) 2 The porous nano material is uniformly distributed like a sphere under a 2 ten thousand times scanning electron microscope (see figure 1 a), 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 the length of 200-500 nm and the width of 30-200 nm in a staggered manner 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 invention 2 O 4 (OH) 2 The 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 down feather interweaved spheroidal carbon and nitrogen doped CaTi prepared by the embodiment of the invention 2 O 4 (OH) 2 Porous nanomaterials, other than CaTi 2 O 4 (OH) 2 The elements Ca, ti and O in the composition, and also C, P, S, N and Pt, are described in CaTi 2 O 4 (OH) 2 A small amount of C and N are doped in the XRD, and trace amounts of P and S are also doped in the XRD, so that the radii of C and N atoms are small, the lattice distortion of the C and N atoms is caused, and an XRD diffraction peak shifts to the right, wherein Pt is caused by platinum-spraying.
As shown in FIG. 4a, the down feather interwoven spheroidal carbon nitrogen doped CaTi prepared by the embodiment of the invention 2 O 4 (OH) 2 A porous nanomaterial having an average pore size of 12.9248nm; BET specific surface area of 510.9175 m as shown in FIG. 4b 2 /g。
As shown in FIG. 5, the velvet interlaced spherical carbon-nitrogen-doped CaTi prepared by the embodiment of the invention 2 O 4 (OH) 2 The 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 invention 2 O 4 (OH) 2 Porous nanomaterial and pure CaTi 2 O 4 (OH) 2 Electrode material at an operating current density of 10mA/cm 2 The specific capacitance of (d) is 1513.1F × g respectively -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/cm 2 When the specific capacitance is pure CaTi 2 O 4 (OH) 2 The 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 doping 2 O 4 (OH) 2 Crystal structure, which is consistent with XRD results.
As shown in FIG. 7, the down feather interweaved spheroidal carbon and nitrogen doped CaTi prepared by the embodiment of the invention 2 O 4 (OH) 2 The 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 CaTi 2 O 4 (OH) 2 The 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 invention 2 O 4 (OH) 2 Porous nanomaterials, CP curves and standardsThe quasi isosceles triangles have certain difference, which is possibly mixed with the down feather to form the quasi-spherical carbon and nitrogen doped CaTi 2 O 4 (OH) 2 The 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 1 2 O 4 (OH) 2 The working current density of the porous nano electrode material is 10mA/cm 2 、20mA/cm 2 、50mA/cm 2 、100mA/cm 2 、200mA/cm 2 The specific capacitances were 1513.1F × g, respectively -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 CaTi 2 O 4 (OH) 2 The 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 and discharge rate of the capacitor. As can also be seen from FIG. 6, the down-feather interlaced spheroidal carbon-nitrogen-doped CaTi 2 O 4 (OH) 2 The porous nano electrode material has uniform CP curve shape, and shows excellent rate capability and charge-discharge performance of the electrode material.
Claims (8)
1. Velvet-interwoven spheroidal carbon-nitrogen-doped CaTi 2 O 4 (OH) 2 The preparation method of the porous nano material is characterized by comprising the following steps:
(1) Soaking the feathers in a chlorine dioxide solution for 18-24 h for disinfection, then washing the disinfected feathers with distilled water for 5-10 times, soaking the feathers in an ethanol solution for 1-2 days for secondary disinfection and carrying out ultrasonic oscillation for 30min, washing the feathers with distilled water for 5-10 times, and naturally drying the feathers at a ventilated place to obtain pretreated feathers; feather, chlorine dioxide solution, distilled water and ethanol in the weight ratio of 1-20 to 1-5 to 500-2000 to 5-50;
(2) Dissolving tetra-n-butyl titanate in ethanol according to the molar ratio of tetra-n-butyl titanate to ethanol = 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 mol ratio of the calcium chloride to the distilled water to the ethanol = 5-25: 300-500: 10-20, then adding the ethanol, stirring and mixing to obtain a solution B;
(4) According to the mol ratio of calcium chloride to tetra-n-butyl titanate = 1: 1-2, adding the solution A into the solution B, 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 CaTi 2 O 4 (OH) 2 A precursor;
(5) According to the mass ratio of CaTi 2 O 4 (OH) 2 The precursor and the pretreated feather are = 1: 0.1-1.2, stirred and mixed, then put into a hydrothermal reaction kettle, kept at the hydrothermal temperature of 160-200 ℃ for 18-30 h, and the reaction product is washed, filtered and dried to obtain the down-feather interweaving spheroidal carbon and nitrogen doped CaTi 2 O 4 (OH) 2 A porous nanomaterial.
2. The velvet interwoven spheroidal carbon nitrogen-doped CaTi as claimed in claim 1 2 O 4 (OH) 2 The preparation method of the porous nano material is characterized by comprising the following steps: the feather is bird feather.
3. The velvet interwoven spheroidal carbon nitrogen-doped CaTi as claimed in claim 1 2 O 4 (OH) 2 The 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.
4. The velvet interwoven spheroidal carbon nitrogen-doped CaTi as claimed in claim 1 2 O 4 (OH) 2 The 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; the stirring and mixing time of the step (5) is 5-20 min.
5. According to claim 1The down feather interweaving spheroidal carbon and nitrogen doped CaTi 2 O 4 (OH) 2 The 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 to 36 hours at the temperature of between 60 and 80 ℃, and the freeze drying is drying for 36 to 48 hours at the temperature of between 30 ℃ below zero and 40 ℃ below zero.
6. Doping CaTi with the feather-interweaving spheroidal carbon-nitrogen according to any of claims 1 to 5 2 O 4 (OH) 2 The product is prepared by the preparation method of the porous nano material.
7. The method of claim 6, wherein the blended carbon and nitrogen CaTi is spherical carbon and nitrogen 2 O 4 (OH) 2 The 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 nano sheets in a staggered manner, the aperture of the micropores is 3-5 nm, and the aperture of the mesopores is 8-30 nm; the length of the nano sheet is 200-500 nm, the width is 30-200 nm, the thickness is less than 30nm, and the long-edge micro-roll is formed.
8. Doping CaTi with the feather-interweaving spheroidal carbon-nitrogen according to any of claims 1 to 5 2 O 4 (OH) 2 The 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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| CN106492865A (en) * | 2016-09-06 | 2017-03-15 | 景德镇陶瓷大学 | A kind of method that 2 composites of C3N4/CaTi2O4 (OH) are prepared using solvent-thermal method |
| CN110950377A (en) * | 2019-12-11 | 2020-04-03 | 景德镇陶瓷大学 | Hydrothermal method and C-embedding firing preparation C-doped CaTi2O4(OH)2Method of nanosheet structure and products thereof |
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| CN102583319A (en) * | 2012-02-28 | 2012-07-18 | 中国科学院长春应用化学研究所 | Nitrogen-doped porous carbon material and preparation method thereof |
| CN104628394A (en) * | 2015-02-14 | 2015-05-20 | 景德镇陶瓷学院 | CaTi2O4(OH)2 cellular powder material and preparation method thereof |
| CN106492865A (en) * | 2016-09-06 | 2017-03-15 | 景德镇陶瓷大学 | A kind of method that 2 composites of C3N4/CaTi2O4 (OH) are prepared using solvent-thermal method |
| CN110950377A (en) * | 2019-12-11 | 2020-04-03 | 景德镇陶瓷大学 | Hydrothermal method and C-embedding firing preparation C-doped CaTi2O4(OH)2Method of nanosheet structure and products thereof |
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