CN112909259A - Method for preparing carbon nanotube material catalytically grown from FeNi alloy by electromagnetic induction heating method - Google Patents
Method for preparing carbon nanotube material catalytically grown from FeNi alloy by electromagnetic induction heating method Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 35
- 229910002555 FeNi Inorganic materials 0.000 title claims abstract description 33
- 239000000463 material Substances 0.000 title claims abstract description 33
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 28
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 28
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 21
- 239000000956 alloy Substances 0.000 title claims abstract description 21
- 238000010438 heat treatment Methods 0.000 title claims abstract description 21
- 230000005674 electromagnetic induction Effects 0.000 title claims abstract description 11
- 230000006698 induction Effects 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 17
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007787 solid Substances 0.000 claims abstract description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000005520 cutting process Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 229910052742 iron Inorganic materials 0.000 claims abstract description 7
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 7
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 239000012300 argon atmosphere Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 8
- VEPSWGHMGZQCIN-UHFFFAOYSA-H ferric oxalate Chemical compound [Fe+3].[Fe+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O VEPSWGHMGZQCIN-UHFFFAOYSA-H 0.000 claims description 5
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 abstract description 6
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 6
- 238000007599 discharging Methods 0.000 abstract description 4
- 238000003860 storage Methods 0.000 abstract description 3
- 239000011669 selenium Substances 0.000 description 10
- 229910014589 Na—Se Inorganic materials 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 229910052711 selenium Inorganic materials 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000012983 electrochemical energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 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 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
-
- 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
Abstract
The invention discloses a method for preparing a carbon nano tube catalytically grown by FeNi alloy by an electromagnetic induction heating method, which comprises the following steps: weighing an iron source, a nickel source and a carbon source according to a proportion, and fully mixing and grinding; placing the mixture in a crucible in an induction alternating magnetic field environment and an inert gas atmosphere, cutting a magnetic induction line by the material, generating induction current, heating, controlling the temperature to be 300-700 ℃, and naturally cooling and collecting a product; step three, standing the product obtained in the step two in nitric acid, corroding 70% of FeNi alloy, separating out residual solid, and drying; step four, mixing the product obtained in the step three with selenium powder in proportion, placing the mixture in a reaction kettle in a sealed glove box under an inert gas atmosphere, heating the mixture to 100-300 ℃ in a homogeneous reaction instrument, and preserving heat for 6-12 hours to obtain a product FeNi @ Se/C; the invention has excellent sodium ion storage performance, high charge-discharge capacity and good rate capability; the conductivity and structural stability of the material in the charging and discharging process can be obviously improved.
Description
Technical Field
The invention belongs to the field of composite material synthesis, relates to preparation of a carbon nanotube material, and particularly relates to a method for preparing a carbon nanotube material catalytically grown by FeNi alloy by an electromagnetic induction heating method.
Background
The application of the electrochemical energy storage technology effectively solves the problems of storage, utilization and conversion of clean energy, and has wide development prospect in the future. At present, lithium ion batteries are widely applied to the field of electrochemical energy storage due to the advantages of excellent performances of the lithium ion batteries, such as high energy density, high energy conversion rate, good safety and the like. However, as research on lithium ion batteries continues, the capacity of lithium ion batteries has been difficult to increase. To meet the demand for ever-evolving large energy storage devices, we are beginning to look at other battery systems. Rechargeable Na-Se batteries are considered to be a promising next generation battery due to their high energy density and low cost. In the Na-Se battery, Se is used as a battery positive electrode, and a sodium sheet is used as a negative electrode. However, the volume expansion of selenium in the charging and discharging process and the shuttle effect of the polyselenide are problems, so that the battery of the system can not reach the theoretical capacity. It is crucial to study a suitable carrier for selenium in Na-Se cells to solve the problems of volume expansion and shuttle effect.
The carbon nano tube is a common soft carbon material, has a good graphitized structure and has excellent conductivity. Meanwhile, the carbon nano tube has good mechanical strength, and the problem of volume expansion and shuttle effect in the charging and discharging reaction process can be effectively inhibited by loading selenium in a one-dimensional network formed by the carbon nano tube. However, the carbon nanotubes themselves have small tube diameters, so that loading selenium in the tubes is difficult, and the carbon nanotubes have few surface defects and are difficult to fix selenium. If the technology can increase the tube diameter of the carbon nano tube by a confinement method, increase the defects and strengthen the fixing capacity of the carbon nano tube to Se element, the application of the material in the field of Na-Se battery electrode materials is expected to be popularized.
Disclosure of Invention
The invention aims to provide a method for preparing a carbon nanotube material catalytically grown by FeNi alloy by an electromagnetic induction heating method, which realizes the controllable in-situ growth of a carbon nanotube by controlling the process conditions in the reaction process and then coordinating with a FeNi alloy catalyst to catalyze the growth of the carbon nanotube.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a carbon nanotube material catalytically grown by FeNi alloy by an electromagnetic induction heating method comprises the following steps:
the method comprises the following steps: weighing an iron source, a nickel source and a carbon source according to a proportion, and fully mixing and grinding;
step two: placing the ground solid powder in a sealed glove box in a crucible under the argon atmosphere, and cutting magnetic induction lines by the materials in the crucible under the induction alternating magnetic field environment to generate induction current, so that the materials in the crucible are heated, the temperature is controlled to be 300-700 ℃, and after the reaction temperature is reached, stopping heating, naturally cooling the product and collecting the product;
step three: standing the product obtained in the step two in nitric acid, corroding for 12 hours, separating out residual solids, and drying;
step four: and (3) mixing the product obtained in the step three with selenium powder in proportion, placing the mixture in a reaction kettle in a sealed glove box under an inert gas atmosphere, heating the mixture to 100-300 ℃ in a homogeneous reactor, and preserving the heat for 6-12 hours to obtain a product FeNi @ Se/C.
Furthermore, the iron source and the nickel source are analytically pure ferric oxalate, ferric oxide, ferric chloride, nickel nitrate, nickel sulfate and nickel chloride.
Further, the carbon source is urea, melamine or glucose.
Further, the weight ratio of the iron source, the nickel source and the carbon source is 1: (6-19): (3-40).
Furthermore, the crucible is a quartz crucible or an alumina crucible.
Further, the inert gas is argon.
Further, the concentration of the nitric acid is 0.5, 1M or 3M.
Further, the weight ratio of the product obtained in the third step to the selenium powder is 1: (1.5-4).
The invention firstly adopts an electromagnetic induction heating method to realize the catalysis of the carbon nano tube by the FeNi alloy, the FeNi alloy is heated under the influence of electromagnetic induction in the process of electromagnetic induction heating, and the carbon around the FeNi alloy is gathered around and grows along a certain direction along with the increase of the temperature, and finally the carbon nano tube is generated. The advantage of utilizing electromagnetic induction heating is that only the FeNi alloy can be heated in the inside, has reduced its self-agglomeration of carbon of periphery to produce the carbon nanotube of more even structure. Washing off excessive FeNi alloy by acid, and finally loading Se by a solid phase to obtain FeNi @ Se/C; the FeNi @ Se/C prepared by the invention has a simple substance Se with higher theoretical capacity, and the FeNi alloy-catalyzed carbon nanotube synthesized by the invention has thicker tube diameter and abundant active sites, so that the load capacity on Se is improved, the FeNi @ Se/C has excellent sodium ion storage performance, high charge-discharge capacity and good rate capability; the highly graphitized tube wall of the carbon tube can obviously improve the conductivity and structural stability of the material in the charging and discharging process.
The raw materials used in the invention are cheap and easily available, and the preparation method is simple.
Drawings
FIG. 1 is a scanning electron micrograph of a sample of example 1
FIG. 2 is an XRD spectrum of a sample of example 1
FIG. 3 is a graph of the cycle performance of the sodium ion battery of the sample of example 1
Detailed Description
Example 1:
the method comprises the following steps: fully grinding 0.1g of ferric oxalate, 0.9g of nickel nitrate and 2g of melamine in a mortar;
step two: placing the ground solid powder in a sealed glove box in a crucible under the argon atmosphere, and cutting magnetic induction lines by the materials in the crucible under the induction alternating magnetic field environment to generate induction current, so that the materials in the crucible are heated, the temperature is controlled at 700 ℃, and the product is obtained after the product is naturally cooled and collected;
step three: standing the obtained product in nitric acid with the concentration of 3M, corroding for 12 hours, separating out residual solid, and drying;
step four: and (3) mixing the product obtained in the step three with selenium powder in a ratio of 2:3, placing the mixture in a reaction kettle in a sealed glove box under an argon atmosphere, heating the mixture to 260 ℃ in a homogeneous reaction instrument, and preserving the heat for 12 hours to obtain FeNi @ Se/C.
Example 2:
the method comprises the following steps: fully grinding 0.05g of ferric oxalate, 0.95g of nickel nitrate and 2g of urea in a mortar;
step two: placing the ground solid powder in a sealed glove box in a crucible under the argon atmosphere, and cutting magnetic induction lines by the materials in the crucible under the induction alternating magnetic field environment to generate induction current, so that the materials in the crucible are heated, the temperature is controlled at 600 ℃, and the product is obtained after the product is naturally cooled and collected; (ii) a
Step three: standing the obtained product in nitric acid with the concentration of 1M, corroding for 12 hours, separating out residual solid, and drying;
step four: and (3) mixing the product obtained in the step three with selenium powder in a ratio of 1:4, placing the mixture in a reaction kettle in a sealed glove box under an argon atmosphere, heating the mixture to 260 ℃ in a homogeneous reaction instrument, and preserving the heat for 12 hours to obtain FeNi @ Se/C.
Example 3:
the method comprises the following steps: 0.3g of iron oxalate, 0.2g of nickel nitrate and 2g of urea are fully ground in a mortar,
step two: placing the ground solid powder in a sealed glove box in a crucible under the argon atmosphere, and cutting magnetic induction lines by the materials in the crucible under the induction alternating magnetic field environment to generate induction current, so that the materials in the crucible are heated, the temperature is controlled at 300 ℃, and the product is obtained after the product is naturally cooled and collected; (ii) a
Step three: standing the obtained product in nitric acid with the concentration of 0.5M, corroding for 12 hours, separating out residual solid, and drying;
step four: and (3) mixing the product obtained in the step three with selenium powder in a ratio of 1:4, placing the mixture in a reaction kettle in a sealed glove box under an argon atmosphere, heating the mixture to 260 ℃ in a homogeneous reaction instrument, and preserving the heat for 10 hours to obtain FeNi @ Se/C.
When the sample prepared in example 1 is observed under a scanning electron microscope, as can be seen from fig. 1, the product is a bamboo-like carbon tube; the product B was analyzed by means of a Japanese science D/max2000 PCX-ray diffractometer, and the XRD of the obtained product 1 is shown in figure 2; preparing the obtained product into a button type sodium ion battery, and specifically packaging the button type sodium ion battery by the following steps: uniformly grinding active powder, a conductive agent (Super P) and a bonding agent (PVDF) according to the mass ratio of 8:1:1 to prepare slurry, uniformly coating the slurry on a copper foil by using a film coater, and drying for 12 hours at 80 ℃ in a vacuum drying oven. And then assembling the electrode plates into a Na-Se battery, performing constant-current charge and discharge test on the battery by adopting a Xinwei electrochemical workstation, wherein the test voltage is 0.01V-3.0V, assembling the obtained material into a button battery, and testing the performance of the sodium-ion battery cathode material, wherein the multiplying power performance is shown in figure 3.
Example 4:
the method comprises the following steps: 1g of ferric oxide, 6g of nickel chloride and 10g of glucose are fully ground in a mortar,
step two: placing the ground solid powder in a sealed glove box in a crucible under the argon atmosphere, and cutting magnetic induction lines by the materials in the crucible under the induction alternating magnetic field environment to generate induction current, so that the materials in the crucible are heated, the temperature is controlled at 300 ℃, and the product is obtained after the product is naturally cooled and collected;
step three: standing the obtained product in nitric acid with the concentration of 0.5M, corroding for 12 hours, separating out residual solid, and drying;
step four: and (3) mixing the product obtained in the step three with selenium powder in a ratio of 1:3, placing the mixture in a reaction kettle in a sealed glove box under an argon atmosphere, heating the mixture to 300 ℃ in a homogeneous reaction instrument, and preserving the heat for 6 hours to obtain FeNi @ Se/C.
Example 5:
the method comprises the following steps: fully grinding 1g of ferric chloride, 12g of nickel sulfate and 3g of glucose in a mortar,
step two: placing the ground solid powder in a sealed glove box in a crucible under the argon atmosphere, and cutting magnetic induction lines by the materials in the crucible under the induction alternating magnetic field environment to generate induction current, so that the materials in the crucible are heated, the temperature is controlled at 500 ℃, and the product is obtained after the product is naturally cooled and collected;
step three: standing the obtained product in nitric acid with the concentration of 0.5M, corroding for 12 hours, separating out residual solid, and drying;
step four: and (3) mixing the product obtained in the step three with selenium powder in a ratio of 1:2, placing the mixture in a reaction kettle in a sealed glove box under an argon atmosphere, heating the mixture to 100 ℃ in a homogeneous reaction instrument, and preserving the heat for 12 hours to obtain FeNi @ Se/C.
Claims (8)
1. A method for preparing a carbon nanotube material catalytically grown by FeNi alloy by an electromagnetic induction heating method is characterized by comprising the following steps:
the method comprises the following steps: weighing an iron source, a nickel source and a carbon source according to a proportion, and fully mixing and grinding;
step two: placing the ground solid powder in a sealed glove box in a crucible under the argon atmosphere, and cutting magnetic induction lines by the materials in the crucible under the induction alternating magnetic field environment to generate induction current, so that the materials in the crucible are heated, the temperature is controlled to be 300-700 ℃, and after the reaction temperature is reached, stopping heating, naturally cooling the product and collecting the product;
step three: standing the product obtained in the step two in nitric acid, corroding for 12 hours, separating out residual solids, and drying;
step four: and (3) mixing the product obtained in the step three with selenium powder in proportion, placing the mixture in a reaction kettle in a sealed glove box under an inert gas atmosphere, heating the mixture to 100-300 ℃ in a homogeneous reactor, and preserving the heat for 6-12 hours to obtain a product FeNi @ Se/C.
2. The method for preparing a carbon nanotube material catalytically grown by FeNi alloy according to claim 1, wherein the iron source and the nickel source are analytically pure iron oxalate, iron oxide, ferric chloride, nickel nitrate, nickel sulfate and nickel chloride.
3. The method for preparing a carbon nanotube material catalytically grown by an FeNi alloy according to claim 1, wherein the carbon source is urea, melamine, or glucose.
4. The method for preparing a carbon nanotube material catalytically grown by an FeNi alloy according to claim 2, wherein the weight ratio of the iron source, the nickel source and the carbon source is 1: (6-19): (3-40).
5. The method for preparing a carbon nanotube material catalytically grown by an FeNi alloy according to claims 2 and 3, wherein the crucible is a quartz crucible or an alumina crucible.
6. The method for preparing a carbon nanotube material catalytically grown by FeNi alloy according to claim 1 wherein the inert gas is argon.
7. The method for preparing a carbon nanotube material catalytically grown by an FeNi alloy according to claim 1 wherein the nitric acid is present at a concentration of 0.5, 1 or 3M.
8. The method for preparing the carbon nanotube material catalytically grown by the FeNi alloy according to claim 1, wherein the weight ratio of the product obtained in the third step to the selenium powder is 1: (1.5-4).
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