CN112909257A - Carbon nanotube material prepared by FeNi alloy catalytic growth through electromagnetic induction heating method and application thereof - Google Patents
Carbon nanotube material prepared by FeNi alloy catalytic growth through electromagnetic induction heating method and application thereof Download PDFInfo
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- 229910002555 FeNi Inorganic materials 0.000 title claims abstract description 43
- 239000000463 material Substances 0.000 title claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 23
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 19
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 16
- 239000000956 alloy Substances 0.000 title claims abstract description 16
- 238000010438 heat treatment Methods 0.000 title claims abstract description 11
- 230000005674 electromagnetic induction Effects 0.000 title claims abstract description 8
- 230000003197 catalytic effect Effects 0.000 title abstract description 5
- 239000011669 selenium Substances 0.000 claims abstract description 19
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002071 nanotube Substances 0.000 claims abstract description 14
- HVAKSLUOHARFLM-UHFFFAOYSA-N selenium;sodium Chemical compound [Se][Na] HVAKSLUOHARFLM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 13
- 239000007790 solid phase Substances 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 230000007547 defect Effects 0.000 claims abstract description 5
- 238000011068 loading method Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 abstract description 5
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 5
- 238000003860 storage Methods 0.000 abstract description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 abstract 1
- 235000017491 Bambusa tulda Nutrition 0.000 abstract 1
- 241001330002 Bambuseae Species 0.000 abstract 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 abstract 1
- 239000011425 bamboo Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 9
- 230000006698 induction Effects 0.000 description 9
- 239000012300 argon atmosphere Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 229910014589 Na—Se Inorganic materials 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 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 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 238000012983 electrochemical energy storage Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000005516 engineering process Methods 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
- 229920000877 Melamine resin Polymers 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000003575 carbonaceous material 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
- 239000006258 conductive agent Substances 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 238000001000 micrograph 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
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- 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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
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Abstract
本发明公开了一种电磁感应加热法制备FeNi合金催化生长的碳纳米管材料及其应用，硒固相负载于内部有缺陷的FeNi/C纳米管材料，FeNi@Se/C纳米管材料为竹节状碳管，FeNi/C与硒的重量比为1:4或2:3，本发明还保护一种含有上述的FeNi@Se/C纳米管材料的钠硒电池正极，以及一种包含上述的钠硒电池正极的钠硒电池；本发明通过Se固相负载在FeNi合金催化的碳纳米管，从而得到FeNi@Se/C，所制备的FeNi@Se/C纳米管材料，具有优异的钠离子存储性能，充放电容量高且倍率性能佳；可显著提升材料在充放电过程中的导电性和结构稳定性。
The invention discloses a carbon nanotube material prepared by an electromagnetic induction heating method for catalytic growth of FeNi alloy and its application. The selenium solid phase is loaded on the FeNi/C nanotube material with internal defects, and the FeNi@Se/C nanotube material is bamboo. Nodular carbon tube, the weight ratio of FeNi/C to selenium is 1:4 or 2:3, the present invention also protects a sodium-selenium battery positive electrode containing the above FeNi@Se/C nanotube material, and a sodium-selenium battery containing the above-mentioned FeNi@Se/C nanotube material. The sodium-selenium battery of the positive electrode of the sodium-selenium battery; the present invention obtains FeNi@Se/C through the solid phase of Se supported on the carbon nanotube catalyzed by the FeNi alloy, and the prepared FeNi@Se/C nanotube material has excellent sodium Ion storage performance, high charge and discharge capacity and good rate performance; can significantly improve the conductivity and structural stability of the material during charge and discharge.
Description
Technical Field
The invention belongs to the technical field of sodium-selenium batteries, relates to a sodium-selenium battery electrode material, and particularly relates to a carbon nano tube material prepared by FeNi alloy catalytic growth through an electromagnetic induction heating method and application thereof.
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 carbon nanotube material prepared by FeNi alloy catalytic growth through an electromagnetic induction heating method and application thereof, so that the battery structure is more stable, the load capacity of the battery is increased, and the multiplying power and the cycle performance of the battery are improved.
In order to realize the purpose, the invention adopts the following technical scheme to realize the purpose:
an electromagnetic induction heating method for preparing a carbon nanotube material catalytically grown from FeNi alloy, wherein selenium is loaded on a FeNi/C nanotube material with defects inside in a solid phase manner.
The invention also has the following technical characteristics:
the FeNi @ Se/C nanotube material is a bamboo-shaped carbon tube.
Preferably, the bamboo-shaped carbon tube is a carbon nanotube grown by FeNi alloy in-situ catalysis, excessive FeNi alloy is removed by acid washing, and a FeNi/C nanotube material is obtained by carrying Se on a solid phase.
Preferably, the weight ratio of FeNi/C to selenium is 1:4 or 2: 3.
The invention also discloses a sodium-selenium battery anode containing the FeNi @ Se/C nanotube material.
The invention also provides a sodium-selenium battery comprising the sodium-selenium battery anode.
The technical effects are as follows:
according to the invention, a carbon nano tube catalyzed by FeNi alloy is loaded by a Se solid phase, so that FeNi @ Se/C is obtained; according to the FeNi @ Se/C nanotube material prepared by the invention, as the structure of the FeNi carbon nanotube is a highly graphitized carbon nanotube, the material loaded with selenium has the advantages of good electron transmission path and high mechanical strength when being used in the charging and discharging processes of the sodium selenium battery, and can improve the conductivity and relieve the influence caused by volume expansion in the charging and discharging processes. And active sites exposed inside the selenium-enriched selenium-. The material has excellent sodium ion storage performance, high charge and discharge capacity and good rate performance; the conductivity and structural stability of the material in the charging and discharging process can be obviously improved.
Furthermore, the raw materials used in the invention are cheap and easy to obtain, and the preparation method is simple.
Drawings
FIG. 1 is a scanning electron microscope image of the FeNi @ Se/C material of the invention
FIG. 2 is an XRD pattern of the FeNi @ Se/C material of the invention
FIG. 3 is a diagram of the cycle performance of a sodium selenium battery prepared from the FeNi @ Se/C material of the invention
The specific implementation mode is as follows:
the preparation method of the FeNi @ Se/C material comprises the following steps:
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;
step three: standing the obtained product in nitric acid with the concentration of 1M, 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 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: 3g of ferric oxalate, 2g of nickel nitrate and 10g 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;
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 12 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.
Claims (6)
1. An electromagnetic induction heating method for preparing a carbon nanotube material catalytically grown from FeNi alloy is characterized in that selenium is loaded on the FeNi/C nanotube material with defects inside in a solid phase manner.
2. The method for preparing a carbon nanotube material catalytically grown by FeNi alloy according to claim 1, wherein the FeNi @ Se/C nanotube material is a bamboo-shaped carbon tube.
3. The method for preparing the carbon nanotube material catalytically grown by the FeNi alloy through the electromagnetic induction heating method according to claim 2, wherein the bamboo-shaped carbon tubes are carbon nanotubes catalytically grown in situ by the FeNi alloy, excessive FeNi alloy is removed through acid washing, and the FeNi/C nanotube material is obtained through solid-phase loading of Se.
4. The method for preparing a carbon nanotube material catalytically grown by FeNi alloy according to claim 3, wherein the weight ratio of FeNi/C to selenium is 1:4 or 2: 3.
5. A sodium selenium cell positive electrode comprising the FeNi @ Se/C nanotube material of any of claims 1 through 4.
6. A sodium selenium battery comprising the sodium selenium battery positive electrode according to claim 5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113991114A (en) * | 2021-10-22 | 2022-01-28 | 陕西科技大学 | Zn-doped Ni-based/carbon nanotube composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113991114A (en) * | 2021-10-22 | 2022-01-28 | 陕西科技大学 | Zn-doped Ni-based/carbon nanotube composite material and preparation method thereof |
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