CN116715228A - Preparation method of sisal fiber carbon anode material with crown-shaped core-shell structure - Google Patents
Preparation method of sisal fiber carbon anode material with crown-shaped core-shell structure Download PDFInfo
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- 244000198134 Agave sisalana Species 0.000 title claims abstract description 61
- 239000000835 fiber Substances 0.000 title claims abstract description 53
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 36
- 239000010405 anode material Substances 0.000 title claims abstract description 22
- 239000011258 core-shell material Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000007773 negative electrode material Substances 0.000 claims abstract description 24
- 229910001415 sodium ion Inorganic materials 0.000 claims abstract description 15
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920000767 polyaniline Polymers 0.000 claims abstract description 11
- 239000007833 carbon precursor Substances 0.000 claims abstract description 8
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 239000002086 nanomaterial Substances 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- GWBWGPRZOYDADH-UHFFFAOYSA-N [C].[Na] Chemical compound [C].[Na] GWBWGPRZOYDADH-UHFFFAOYSA-N 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 229910001220 stainless steel Inorganic materials 0.000 claims 1
- 239000010935 stainless steel Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 230000001351 cycling effect Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 239000002121 nanofiber Substances 0.000 abstract 1
- 235000011624 Agave sisalana Nutrition 0.000 description 7
- 239000002002 slurry Substances 0.000 description 6
- 238000002484 cyclic voltammetry Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 239000011889 copper foil Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 239000002114 nanocomposite Substances 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- 238000001237 Raman spectrum Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000006230 acetylene black Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 101150047356 dec-1 gene Proteins 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000004080 punching Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/18—Nanoonions; Nanoscrolls; Nanohorns; Nanocones; Nanowalls
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
- H01M4/602—Polymers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of a sisal fiber carbon (PAN-SSFC) negative electrode material with a crown core-shell structure, which is characterized in that in the preparation process of PAN-SSFC, a two-step method (hydrothermal reaction and high-temperature calcination) is utilized to prepare a sisal fiber carbon material (SSFC) with a smooth and uniform spherical morphology, and then a surface coating method is utilized to uniformly coat polymerized polyaniline nanofiber on the surface of the SSFC, so that the sisal fiber carbon nanocomposite-structure sodium ion battery negative electrode material with the crown core-shell structure is obtained. The preparation process is simple, energy-saving and environment-friendly; the sisal fiber is used as a carbon precursor, has the characteristics of wide source, stable structure and high fiber content, and the PAN-SSFC anode material obtained by regulating and controlling the morphology and structure of sisal fiber carbon has an obvious charge and discharge platform, so that the cycling stability of a sodium ion battery can be effectively enhanced, and the electrochemical performance is improved.
Description
Technical Field
The invention relates to a preparation method of a sisal fiber carbon negative electrode material with a crown-shaped core-shell structure, belonging to the fields of sodium ion battery electrode materials and biomass charcoal.
Background
With the advent of the smart grid era, energy storage battery systems have become popular in research in recent years. Sodium ion batteries are widely focused by researchers at home and abroad due to the advantages of low cost, high safety, abundant resources and the like, become the battery system with the most development potential, and are expected to be applied to large-scale energy storage systems in the future. However, the progress of the practical use of sodium ion batteries is still limited by the lack of a negative electrode material that is excellent in performance and practical. For the anode material, the granularity, the morphology, the structure, the specific surface area and the like of the anode material have important influences on the electrochemical performance of the anode material, so that the anode material has important significance in regulating and controlling the morphology and the structure of the anode material.
Biomass charcoal is a porous solid particulate matter with high aromaticity and rich carbon, which is produced by thermochemical conversion of biomass rich in carbon under anaerobic or anoxic conditions. As a renewable carbon material, the material has rich pore structure, larger specific surface area and more oxygen-containing active groups on the surface, and is a multifunctional material with excellent performance. Sisal hemp is used as a representative of Guangxi special agricultural plants, is rich in sources, has high content of cellulose, lignin and the like, and can effectively accelerate the practical process of the sodium ion battery by taking sisal hemp fiber as a precursor to prepare a high-performance sisal hemp fiber carbon negative electrode material with specific morphology and structure.
The invention creatively uses the sisal fiber carbon nano composite structure with the crown-shaped core-shell structure to prepare the negative electrode material of the sodium ion battery, the inner core of the sisal fiber carbon negative electrode material with the crown-shaped core-shell structure is a uniform spherical sisal fiber carbon material, the outer shell is a polyaniline nano structure material with a crown-shaped appearance, and the sisal fiber carbon negative electrode material with the crown-shaped core-shell structure shows obvious charge and discharge platform, good cycle stability and other electrochemical performances, and compared with pure spherical sisal fiber carbon with a non-nano composite structure, the initial charge and discharge specific capacity of the sisal fiber carbon nano composite structure can be respectively improved by 2-3.4 times and 1-1.5 times under the current density of 100 mA/g.
Disclosure of Invention
The invention aims to provide a preparation method of a crown-shaped core-shell structure sisal fiber carbon serving as a negative electrode material applied to a sodium ion battery. The technology of the invention enables the Guangxi special agricultural plant sisal hemp to be a sodium ion battery carbon precursor, and provides a new way for the resource utilization of sisal hemp.
The technical scheme of the invention is as follows:
1. the technological process of applying sisal carbon with crown-shaped core-shell structure as negative electrode material in sodium ion battery includes the following steps:
(1) Pretreatment of sisal fibers. And selecting sisal fibers, manually rubbing, screening and washing with a screen to remove surface impurities, then cleaning the sisal fibers with deionized water, and putting into a blast drying oven for drying.
(2) Weighing 4-6 g of clean sisal fiber obtained in step (1), shearing into 1-2 cm, and placing into a container containing 65 ml HCl (2 mol. L) -1 ) The solution is subjected to hydrothermal reaction in a polytetrafluoroethylene reaction kettle, and the parameters are set to be 180-190 ℃ and 12-16 h.
(3) And (3) carrying out suction filtration on the suspension obtained in the step (2) (using medium-speed filter paper with the aperture of 9 cm), and washing with deionized water for three times to obtain a black solid precipitate. 60. Drying 24 deg.C and h to obtain sisal fiber carbon precursor, placing sisal fiber carbon precursor into crucible, and calcining at high temperature (N) 2 Atmosphere, 900 ℃,1, h), taking out a black sample in the crucible after natural cooling, and naming the black sample as Spherical Sisal Fiber Carbon (SSFC).
(4) Weighing 1.0-1.5. 1.5 g and 70 ml of H of SSFC prepared in the step (3) 2 SO 4 (1.5 mol•L -1 ) Magnetically stirring for 15 min to obtain dispersed SSFC, adding 0.7-1.5. 1.5 ml aniline (analytically pure) and magnetically stirring for 2H to obtain aniline SSFC, dissolving ammonium persulfate 1.2-1.5. 1.5 g in 8-12 ml H 2 SO 4 (1.5 mol•L -1 ) The formed mixed solution is added into aniline SSFC solution drop by drop, stirred at room temperature for 12 h to obtain polyaniline SSFC solution, the polyaniline SSFC solution is subjected to suction filtration (using medium-speed filter paper with the pore diameter of 9 cm), and is alternately washed with deionized water and absolute ethyl alcoholAnd (3) obtaining a green solid precipitate for three times, and drying the precipitate in an oven at 60 ℃ for 10 h to obtain the carbon sisal fibers with the crown-shaped core-shell structure, which is named as sisal fiber carbon with the crown-shaped core-shell structure (PAN-SSFC).
(5) Mixing the SSFC anode material obtained in the step (3) as a comparison and the PAN-SSFC anode material obtained in the step (4) with acetylene black and polyvinylidene fluoride respectively according to the mass ratio of 8:1:1, preparing slurry by using N-methyl pyrrolidone as a solvent, coating the slurry on copper foil with the thickness of 9 mu m, and drying the slurry in a vacuum drying oven at 110 ℃ for 10 h. After cooling to normal temperature, the copper foil is punched into a round pole piece with the diameter of 16 mm by a sheet punching machine.
(6) The metal sodium sheet is used as a counter electrode, the diaphragm is made of glass fiber, and the electrolyte is 1M NaClO 4 And (EC: DEC 1:1 volume ratio), assembling the solution into a CR2032 type battery in a glove box protected by argon, sealing, standing for 10 h, and performing electrochemical performance test, wherein the test voltage is 3-0.01V, and the current density is 100 mA/g.
The preparation method of the PAN-SSFC as the negative electrode material of the sodium ion battery has the following obvious characteristics:
(1) The raw material sisal hemp is a Guangxi special agricultural plant and has wide sources.
(2) The preparation method has the advantages of simple steps, low raw material cost, energy conservation and environmental protection.
(3) The technology of the invention enables the Guangxi special agricultural plant sisal hemp to be prepared into the negative electrode material PAN-SSFC of the sodium ion battery, the inner core of the PAN-SSFC negative electrode material is a smooth and uniform spherical sisal hemp carbon material, the outer shell is a polyaniline nano-structure material with the crown shape, the thickness of which is only 30-50 nm, and the crown bulge of which is about 50-80 nm, and the PAN-SSFC negative electrode material shows an obvious charge and discharge platform and good cycle stability, thereby providing a new approach for the resource utilization of sisal hemp.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of a spherical sisal fiber carbon anode material obtained in example 1 of the present invention.
FIG. 2 is a Scanning Electron Microscope (SEM) image of a sisal fiber carbon anode material of a crown-type core-shell structure obtained in example 1 of the present invention.
FIG. 3 is an X-ray diffraction (XRD) pattern of a sisal fiber carbon negative electrode material having a crown-type core-shell structure obtained in example 1 of the present invention.
FIG. 4 is a Raman spectrum (Raman) of the carbon negative sisal fiber electrode material with the crown-shaped core-shell structure obtained in example 1 of the present invention.
FIG. 5 is an Electrochemical Impedance (EIS) diagram of a carbon negative sisal fiber electrode material with a crown-type core-shell structure obtained in example 1 of the present invention.
FIG. 6 is a Cyclic Voltammetry (CV) diagram of sisal fiber carbon anode material with a crown-shaped core-shell structure obtained in example 1 of the present invention.
FIG. 7 is a graph showing the cycle performance of the sisal carbon anode material with a crown-type core-shell structure obtained in example 1 of the present invention at a current density of 100 mA/g.
Detailed Description
Example 1:
(1) Pretreatment of sisal fibers. And selecting sisal fibers, manually rubbing, screening and washing with a screen to remove surface impurities, then cleaning the sisal fibers with deionized water, and putting into a blast drying oven for drying.
(2) Weighing 4-6 g of clean sisal fiber obtained in step (1), shearing into 1-2 cm, and placing into a container containing 65 ml HCl (2 mol. L) -1 ) The solution is subjected to hydrothermal reaction in a polytetrafluoroethylene reaction kettle, and the parameters are set to be 180-190 ℃ and 12-16 h.
(3) And (3) carrying out suction filtration on the suspension obtained in the step (2) (using medium-speed filter paper with the aperture of 9 cm), and washing with deionized water for three times to obtain a black solid precipitate. 60. Drying 24 deg.C and h to obtain sisal fiber carbon precursor, placing sisal fiber carbon precursor into crucible, and calcining at high temperature (N) 2 Atmosphere, 900 ℃,1, h), taking out a black sample in the crucible after natural cooling, and naming the black sample as Spherical Sisal Fiber Carbon (SSFC).
(4) Weighing 1.0-1.5. 1.5 g and 70 ml of H of SSFC prepared in the step (3) 2 SO 4 (1.5 mol•L -1 ) Magnetically stirring for 15 min to obtain dispersed SSFC, adding 0.7-1.5. 1.5 ml aniline (analytically pure) and magnetically stirring for 2 h to obtain aniline SSFC,1.2-1.5. 1.5 g ammonium persulfate was dissolved in 8-12 ml of H 2 SO 4 (1.5 mol•L -1 ) The formed mixed solution is added into aniline SSFC solution drop by drop, stirring is carried out at room temperature for 12 h, polyaniline SSFC solution is obtained, suction filtration is carried out on the polyaniline SSFC solution (medium-speed filter paper is used, the aperture is 9 cm), deionized water and absolute ethyl alcohol are used for washing for three times alternately, thus obtaining a green solid precipitate, and oven drying is carried out at 60 ℃ for 10 h to obtain sisal fiber carbon with a crown core-shell structure, and the carbon is named as sisal fiber carbon with a crown core-shell structure (PAN-SSFC).
(5) Mixing the SSFC anode material obtained in the step (3) and the PAN-SSFC anode material obtained in the step (4) with acetylene black and polyvinylidene fluoride respectively according to the mass ratio of 8:1:1, preparing slurry by using N-methyl pyrrolidone as a solvent, coating the slurry on copper foil with the thickness of 9 mu m, and drying the slurry in a vacuum drying oven at 110 ℃ for 10 h. After cooling to normal temperature, the copper foil is punched into a round pole piece with the diameter of 16 mm by a sheet punching machine.
(6) The metal sodium sheet is used as a counter electrode, the diaphragm is made of glass fiber, and the electrolyte is 1M NaClO 4 And (EC: DEC 1:1 volume ratio), assembling the solution into a CR2032 type battery in a glove box protected by argon, sealing, standing for 10 h, and performing electrochemical performance test, wherein the test voltage is 3-0.01V, and the current density is 100 mA/g.
Observing the morphology of the SSFC obtained in the step (3) and the PAN-SSFC obtained in the step (4) by using a scanning electron microscope, wherein the SSFC is of a solid spherical structure with a smooth surface, the particle size of the SSFC is about 3 mu m, and the scanning electron microscope of the PAN-SSFC is shown in FIG. 2, the surface of the PAN-SSFC is coated by a coronary polyaniline nano structure, the height of the coronary bulge is about 50-80 nm, the coating thickness is 30-50 nm, and the inside of the PAN-SSFC is of the solid spherical structure; analysis of the structure of PAN-SSFC, whose XRD patterns are shown in FIG. 3, showed two main broad peaks at about 22℃and 44℃corresponding to (002) and (101) crystal planes, respectively, revealed that the PAN-SSFC sample was an amorphous structure with a lattice spacing d 002 A good sodium storage environment is provided for 0.38 nm, which is located in the optimal layer spacing range (0.37-0.42 nm) of the hard carbon; the Raman spectrum of PAN-SSFC is shown in FIG. 4, which shows two independent characteristic peaks, namelyIs 1340-1340 cm -1 D peak sum-1590 cm -1 G peaks of (2) respectively correspond to having sp 3 Defective D-band and ordered graphite sp 2 The characteristic G band shows that PAN-SSFC has more defects and can provide more active sites for sodium storage; as shown in FIG. 5, the alternating current impedance diagram of the PAN-SSFC anode material has a resistance of about 470 omega, and the PAN-SSFC anode material is beneficial to improving sodium ion transmission compared with 900 omega resistance of the SSFC anode material; cyclic voltammetry CV test As shown in FIG. 6, the PAN-SSFC anode material was scanned at a rate of 0.1 mV s -1 The CV curves of the first three circles are gradually overlapped, and the CV curves of the SSFC negative electrode materials are compared, so that the electrochemical reaction inside the PAN-SSFC negative electrode materials is a reversible reaction and has good cycling stability; the electrochemical performance is shown in figure 7, the initial charge and discharge specific capacities of the PAN-SSFC negative electrode material are 232.2 mAh/g and 656.6 mAh/g respectively, compared with the initial charge and discharge specific capacities of 53.3 and 259.2 mAh/g of the SSFC negative electrode material, the initial charge and discharge specific capacities of the PAN-SSFC are 4.4 times and 2.5 times of the SSFC respectively, namely, the initial charge and discharge specific capacities are respectively improved by 3.4 times and 1.5 times, an obvious charge and discharge platform is provided, the reversible specific capacity of the PAN-SSFC negative electrode material after 170 times of circulation is 157.3 mAh/g, and the reversible specific capacity (72.1 mAh/g) of the PAN-SSFC negative electrode material is obviously superior to that of the SSFC negative electrode material, and the PAN-SSFC negative electrode material has better electrochemical performance is shown.
Claims (2)
1. A preparation method of a sisal fiber carbon (PAN-SSFC) sodium ion battery anode material with a crown-shaped core-shell structure is characterized by comprising the following specific steps:
(1) Pretreatment of sisal fibers; manually rubbing sisal fibers, screening and washing with a stainless steel screen to remove surface impurities, then cleaning the sisal fibers with deionized water, and putting into a blast drying oven for drying;
(2) Weighing 4-6 g of clean sisal fiber obtained in step (1), shearing into 1-2 cm, and placing into a container containing 65 ml HCl (2 mol. L) -1 ) Carrying out hydrothermal reaction in a polytetrafluoroethylene reaction kettle of the solution, wherein the parameters are set to be 180-190 ℃ and 12-16 h;
(3) Suspending the suspension obtained in the step (2)Filtering the turbid liquid (using medium-speed filter paper with the aperture of 9 cm), and washing with deionized water for three times to obtain black solid precipitate; 60. drying 24 deg.C and h to obtain sisal fiber carbon precursor, placing sisal fiber carbon precursor into crucible, and calcining at high temperature (N) 2 Atmosphere, 900 ℃,1, h), taking out a black sample in the crucible after natural cooling, and naming the black sample as Spherical Sisal Fiber Carbon (SSFC);
(4) Weighing 1.0-1.5. 1.5 g and 70 ml of H of SSFC prepared in the step (3) 2 SO 4 (1.5 mol•L -1 ) Magnetically stirring for 15 min to obtain dispersed SSFC, adding 0.7-1.5. 1.5 ml aniline (analytically pure) and magnetically stirring for 2H to obtain aniline SSFC, dissolving ammonium persulfate 1.2-1.5. 1.5 g in 8-12 ml H 2 SO 4 (1.5 mol•L -1 ) The formed mixed solution is added into aniline SSFC solution drop by drop, stirring is carried out at room temperature for 12 h, polyaniline SSFC solution is obtained, suction filtration is carried out on the polyaniline SSFC solution (medium-speed filter paper is used, the aperture is 9 cm), deionized water and absolute ethyl alcohol are used for washing for three times alternately, thus obtaining a green solid precipitate, and drying is carried out in a 60 ℃ oven for 10 h, thus obtaining sisal fiber carbon (PAN-SSFC) anode material with a crown-shell structure.
2. The negative electrode material of the sisal fiber carbon sodium ion battery with the coronary core-shell structure, which is characterized in that the inner core of the PAN-SSFC is a smooth and uniform spherical sisal fiber carbon material, and the outer shell is a polyaniline nano-structure material with a coronary morphology.
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| CN117334886B (en) * | 2023-12-01 | 2024-03-19 | 广东容钠新能源科技有限公司 | Preparation method and application of polyaniline in-situ coated hard carbon material |
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