CN111082040A - Core-shell structure T-Nb2O5Preparation method and application of @ C composite material - Google Patents
Core-shell structure T-Nb2O5Preparation method and application of @ C composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 239000011258 core-shell material Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000002360 preparation method Methods 0.000 claims abstract description 30
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 22
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 21
- 229910019804 NbCl5 Inorganic materials 0.000 claims abstract description 19
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 16
- 239000000661 sodium alginate Substances 0.000 claims abstract description 16
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 16
- 238000004108 freeze drying Methods 0.000 claims abstract description 9
- 239000010405 anode material Substances 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000003763 carbonization Methods 0.000 claims abstract description 5
- 238000010000 carbonizing Methods 0.000 claims abstract description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 239000000758 substrate Substances 0.000 abstract description 3
- 239000010955 niobium Substances 0.000 description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 239000000047 product Substances 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 11
- 229910021641 deionized water Inorganic materials 0.000 description 11
- 238000003756 stirring Methods 0.000 description 9
- 239000002243 precursor Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000010410 layer Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 5
- 238000004729 solvothermal method Methods 0.000 description 5
- QCVGEOXPDFCNHA-UHFFFAOYSA-N 5,5-dimethyl-2,4-dioxo-1,3-oxazolidine-3-carboxamide Chemical compound CC1(C)OC(=O)N(C(N)=O)C1=O QCVGEOXPDFCNHA-UHFFFAOYSA-N 0.000 description 3
- 102000002322 Egg Proteins Human genes 0.000 description 3
- 108010000912 Egg Proteins Proteins 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 235000014103 egg white Nutrition 0.000 description 3
- 210000000969 egg white Anatomy 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
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- 238000006460 hydrolysis reaction Methods 0.000 description 2
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- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000012298 atmosphere Substances 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
- 150000001768 cations Chemical class 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
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- 239000012467 final product Substances 0.000 description 1
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- 239000007769 metal material Substances 0.000 description 1
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- 229910000484 niobium oxide Inorganic materials 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- ZDYUUBIMAGBMPY-UHFFFAOYSA-N oxalic acid;hydrate Chemical compound O.OC(=O)C(O)=O ZDYUUBIMAGBMPY-UHFFFAOYSA-N 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
-
- 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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
-
- 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
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
Abstract
The invention discloses a core-shell structure T-Nb2O5A preparation method and application of a @ C composite material belong to the field of material preparation and application of lithium ion battery anode materials. The invention adds sodium alginate into NbCl5Obtaining a cross-linked product by hydrochloric acid solution, filtering the cross-linked product, freeze-drying and carbonizing at a certain high temperature to prepare the T-Nb with the core-shell structure2O5@ C composite material. The invention uses sodium alginate to provide a carbon substrate, has mesopores with various diameters after carbonization, and is wrapped by T-Nb2O5Combining good electrical conductivity of porous carbon and T-Nb2O5Excellent electrochemical performance. The preparation method is simple, the process is easy to control, the cost is low, and the preparation method is suitable for being used as a material with rapid charge and discharge performanceA lithium ion battery.
Description
Technical Field
The invention belongs to the field of material preparation and application of lithium ion battery anode materials, and particularly relates to T-Nb with a core-shell structure2O5A preparation method and application of the @ C composite material.
Background
With the continuous progress of global industrialization, the demand of human society for energy is continuously increasing. However, in the current energy consumption structure, the proportion of the traditional fossil energy exceeds 80 percent, which causes the problem of limited global reserves on one hand and brings serious environmental pollution problems to the world on the other hand. Based on this, the global research on how to increase the utilization ratio of clean energy sources, such as wind energy, solar energy, tidal energy, etc. However, the utilization of clean energy has certain problems, such as being influenced by environmental factors, for example, the utilization of solar energy can only be performed in the daytime when the illumination condition is satisfied, so the development of energy storage devices is receiving more and more attention. The most widely applied energy storage devices at present are lithium ion batteries and super capacitors, generally, the lithium ion batteries have the characteristics of high energy density and low power density, the super capacitors are just the opposite, and under the requirement of diversified power storage, the novel lithium ion battery device with the advantages of the super capacitors, namely, the novel lithium ion battery device with high energy density and high power density, has huge development space.
In recent years, transition metal oxides having a multi-layer structure, in which a certain interlayer distance may be relatively wide, have been widely studied and spotlighted as an anode material for a lithium ion battery because lithium ions are intercalated and deintercalated therein at a very fast rate. Nb2O5As a member of transition metal oxide having a multi-layer structure, its T-type structure has 4g layers andand 4h layer and 4g layer atoms are arranged sparsely, and lithium ions can be rapidly inserted and separated in the layer, so that the lithium ion battery can be applied to novel lithium ion batteries. But Nb2O5The conductivity is poor, so that the lithium ion battery material needs to be combined with conductive metal or non-metal materials.
Literature describes T-Nb2O5The preparation of the compound is mainly a solvothermal method, such as in-situ growth of T-Nb on a titanium substrate2O5[Wang X,Lee P S.Titanium doped niobium oxide for stablepseudocapacitive lithium ion storage and its application in 3V non-aqueoussupercapacitors[J].Journal of Materials Chemistry A,2015,3(43):21706-21712.]Solvothermal synthesis of T-Nb2O5Carbon composite [ Lim E, Jo C, Kim H, et al. simple synthesis of Nb2O5@ carbon core-shell nanocrystals with controlled crystalline structure for high-power antibodies in hybrid supercapacitors [ J].ACS nano,2015,9(7):7497-7505.]Solvothermal method for growing self-supporting T-Nb on graphene2O5Graphene composite [ Sun H, Mei L, Liang J, et al, three-dimensional holey-graphene/NIOBIA composite amorphous architecture for ultra-high-rate energy storage [ J].Science,2017,356(6338):599-604.]And the like.
T-Nb is prepared by a plurality of researchers2O5The preparation conditions are harsh, and the process is complex: due to Nb5+The preparation process of the researches needs to avoid the contact with water as much as possible, the reaction needs to be carried out under the ice-bath condition by using water as a solvent, and then the synthesis is carried out by a solvothermal method. On the one hand, the anhydrous environment is high in requirement and difficult to obtain, and Nb is inhibited by ice bath5+Hydrolysis has large uncertainty, and on the other hand, the reaction of the solvothermal method is extremely difficult to control and has poor repeatability. Chinese patent application with publication number CN109767925A discloses a T-Nb2O5The preparation method of the/egg white carbon composite material comprises the steps of adding ammonium niobate oxalate hydrate into deionized water, mixing with egg white, dropwise adding HCl, carrying out hydrothermal reaction to obtain a precursor, and carbonizing to obtain T-Nb2O5The composite material is egg white carbon. Such asThe preparation method does not pass through ice bath, is compounded with natural carbon, has better innovation, but still has certain defects, such as the preparation process still needs a hydrothermal reaction process, the uncertainty of the reaction process is higher, the control is extremely difficult, and Nb in the final product is very difficult2O5The content is only 58.3%, and the specific capacity of the whole battery system can be reduced in application. The invention utilizes the self-crosslinking characteristic of sodium alginate and metal ions to prepare T-Nb in the presence of water at normal temperature2O5@ C composite, Nb in final composite2O5A specific gravity of 85.5% provides more active species for the same mass of electrode material. The preparation process of the method is simple and easy to control, has strong repeatability, and has good application in the anode material of the lithium ion battery.
Disclosure of Invention
The invention aims to solve the problem of the existing T-Nb2O5The defects of the material preparation technology provide a core-shell structure T-Nb2O5A preparation method and application of the @ C composite material. The invention is realized by adding excess NbCl5Dissolving in hydrochloric acid solution to inhibit Nb5+Adding sodium alginate which can generate cross-linking reaction with metal cations to form a product with a core-shell structure, cross-linking to obtain a precursor product, and filtering, freeze-drying and high-temperature carbonizing to obtain the T-Nb with the core-shell structure2O5A composite material. The method has the advantages of simple preparation process, easily controlled process and low cost, and is suitable for being used as a lithium ion battery with the rapid charge and discharge performance.
The purpose of the invention is realized by the following technical scheme:
the invention relates to a core-shell structure T-Nb2O5The preparation method of the @ C composite material comprises the steps of firstly adding sodium alginate solution into NbCl5Obtaining a cross-linked product in a hydrochloric acid solution, filtering and freeze-drying the cross-linked product, and carbonizing the cross-linked product at a preset temperature in a nitrogen atmosphere to obtain the core-shell structure T-Nb2O5@ C composite material.
Further, the mass concentration of the sodium alginate solution is 1-2%.
Further, the NbCl5The hydrochloric acid solution is prepared by adding excessive NbCl5Dissolving in hydrochloric acid solution with concentration of 0.5-1mol/L for inhibiting Nb5+And (4) hydrolyzing.
Further, NbCl5In NbCl5The concentration of the hydrochloric acid solution is 0.05-0.15 mol/L.
Further, the sodium alginate solution is mixed with NbCl5The volume ratio of the hydrochloric acid solution is 3: 10-6: 10, preferably 2:5, and the hydrochloric acid solution is stirred for 24-48 hours after mixing.
Further, the filtration is 2-5 times by using deionized water and absolute alcohol respectively.
Further, the freeze drying is carried out for 24-48h under the condition of 1Pa, -60-50 ℃. The aim is to maintain the microstructure of the crosslinked product.
Further, the carbonization is carried out at high temperature under the nitrogen atmosphere, the carbonization temperature is 600-700 ℃, the temperature rise rate is 5-10 ℃/min, preferably 5 ℃/min, the heat preservation time is 2-3 h, and the nitrogen flow rate is 0.6-0.8L/min.
The invention also relates to a core-shell structure T-Nb prepared by the method2O5The application of the @ C composite material in the application of the anode material of the lithium ion battery with the rapid charge and discharge performance.
Compared with the prior art, the invention has the following beneficial effects:
1) the raw materials used in the invention are easy to obtain, the preparation method is simple, the process is easy to control, the cost is low, and the preparation method has good application prospect in the field of lithium ion batteries;
2) the core-shell structure T-Nb prepared by the invention2O5The @ C composite material has excellent characteristics such as good conductivity and charge-discharge rate block;
3) core-shell structure T-Nb prepared by the invention2O5@ C composite material prepared by reacting NbCl5Dissolving in hydrochloric acid solution to inhibit Nb5+The hydrolysis of ions solves the problem of Nb2O5The conventional preparation process is complicated by anhydrous solvothermal reactionThe preparation process is carried out;
4) the invention prepares T-Nb under the conditions of water environment and normal temperature in the reaction process2O5The method also provides a concept for preparing the oxide/carbon composite material under the carbon substrate of other easily hydrolyzed ions.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 shows core-shell T-Nb structure prepared in example 12O5The XRD pattern of @ C composite;
FIG. 2 is core-shell structure T-Nb prepared in example 12O5The transmission and selected area diffraction patterns of the @ C composite material under different resolutions; wherein a is a transmission diagram under the magnification of 2 ten thousand times; b is a transmission image under the magnification of 5 ten thousand times; c is a transmission image under the magnification of 10 ten thousand times; d is a high-resolution transmission image under the magnification of 60 ten thousand times, and the middle inset image is a selected area diffraction image;
FIG. 3 is core-shell structure T-Nb prepared in example 12O5The rate performance graph of the @ C composite material as the anode material of the lithium ion half cell;
FIG. 4 is core-shell structure T-Nb prepared in example 12O5The thermal weight loss curve of the @ C composite material in the air shows that the weight of the carbon in the composite material is rapidly reduced at the temperature of 400-500 ℃ and the oxygen in the air generates combustion reaction, and the sample quality is stable after the temperature of 500 ℃, and is mainly formed by Nb in the composite material2O5Provided is a method.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The embodiment relates to a core-shell structure T-Nb2O5A preparation method of the @ C composite material comprises the following steps:
step one, dissolving 15g of sodium alginate in 985ml of deionized water, stirring for 24 hours, and standing for 24 hours;
step two, adding 17ml of concentrated hydrochloric acid into 383ml of deionized water, and stirring for 15 min;
step three, taking 10g of NbCl5Dissolving in hydrochloric acid solution, and stirring for 15 min;
step four, taking 160ml of sodium alginate solution, and slowly adding NbCl5Hydrochloric acid solution is stirred and cross-linked for 24 hours;
step five, respectively pumping and filtering the product obtained in the step four by using deionized water and absolute ethyl alcohol, and repeatedly treating twice by using the method;
putting the precursor obtained in the fifth step into a freeze dryer, and freeze-drying for 48 hours under the condition of 1 Pa-60 ℃;
step seven, putting the freeze-dried precursor in the step six into a vacuum tube furnace, heating to 600 ℃ at the speed of 5 ℃/min under the nitrogen atmosphere with the flow rate of 0.6-0.8L/min, preserving heat for 2h, and cooling to room temperature to finally obtain the T-Nb with the core-shell structure2O5@ C composite product.
FIG. 1 shows the core-shell structure T-Nb obtained in this example2O5The XRD pattern of the @ C composite; the characteristic crystal face of (181) in FIG. 1 shows that the synthesized product is T-Nb2O5。
FIG. 2 shows the core-shell structure T-Nb obtained in this example2O5Transmission and selected area diffraction patterns for the @ C composite; it can be seen from FIGS. 2(a) and 2(b) that the product synthesized by this method is uniform, and Nb is2O5Has a particle diameter of about 5 to 10nm, and Nb is shown in FIG. 2(c)2O5The particles were coated with carbon, and it was found from FIG. 2(d) that the lattice spacing was 0.31nm, which corresponds to the (180) plane.
FIG. 3 shows the core-shell structure T-Nb obtained in this example2O5The electrochemical performance graph of the @ C composite material as the anode material of the lithium ion half cell; as can be seen from FIG. 3, the current density was 0.05AThe specific capacity per gram is about 150mAh/g, and the specific capacity is about 50mAh/g when the current density is 5A/g.
FIG. 4 shows the core-shell structure T-Nb obtained in this example2O5The thermal weight loss curve of the @ C composite material in the air atmosphere shows that Nb in the composite material2O5The mass ratio of the oxide was 85.5%.
Example 2
The embodiment relates to a preparation method of a T-Nb2O5@ C composite material with a core-shell structure, which comprises the following steps:
step one, dissolving 15g of sodium alginate in 985ml of deionized water, stirring for 24 hours, and standing for 24 hours;
step two, adding 34ml of concentrated hydrochloric acid into 366ml of deionized water, and stirring for 15 min;
step three, taking 15g of NbCl5Dissolving in hydrochloric acid solution, and stirring for 15 min;
step four, taking 200ml of sodium alginate solution, and slowly adding NbCl5Hydrochloric acid solution is stirred and subjected to crosslinking reaction for 48 hours;
step five, respectively pumping and filtering the product obtained in the step four by using deionized water and absolute ethyl alcohol, and repeatedly treating twice by using the method;
putting the precursor obtained in the fifth step into a freeze dryer, and freeze-drying for 48 hours under the condition of 1 Pa-60 ℃;
step seven, putting the freeze-dried precursor in the step six into a vacuum tube furnace, heating to 600 ℃ at the speed of 5 ℃/min under the nitrogen atmosphere with the flow rate of 0.6-0.8L/min, preserving heat for 2h, and cooling to room temperature to finally obtain the T-Nb2O5@ C composite material.
Example 3
The embodiment relates to a preparation method of a T-Nb2O5@ C composite material with a core-shell structure, which comprises the following steps:
step one, dissolving 20g of sodium alginate in 980ml of deionized water, stirring for 24 hours, and standing for 24 hours;
step two, adding 20ml of concentrated hydrochloric acid into 380ml of deionized water, and stirring for 15 min;
step three, taking 10g of NbCl5Dissolving in hydrochloric acid solution, and stirring for 15 min;
step four, taking 160ml of the sodium alginate solution prepared in the step one, and slowly adding NbCl5Hydrochloric acid solution is stirred and subjected to crosslinking reaction for 48 hours;
step five, respectively pumping and filtering the product obtained in the step four by using deionized water and absolute ethyl alcohol, and repeatedly treating twice by using the method;
putting the precursor obtained in the fifth step into a freeze dryer, and freeze-drying for 48 hours under the condition of 1 Pa-60 ℃;
step seven, putting the freeze-dried precursor in the step six into a vacuum tube furnace, heating to 700 ℃ at the speed of 5 ℃/min under the nitrogen atmosphere with the flow rate of 0.6-0.8L/min, preserving heat for 2h, and cooling to room temperature to finally obtain the core-shell structure T-Nb2O5@ C composite product.
Specific examples of the invention are described above. It should be understood that the above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any changes and modifications made to the above technical scheme according to the technical essence of the present invention are all protection contents of the technical scheme of the present invention, unless the contents depart from the technical scheme of the present invention.
Claims (8)
1. Core-shell structure T-Nb2O5A preparation method of a @ C composite material is characterized in that,
adding sodium alginate solution into NbCl5Obtaining a cross-linked product in a hydrochloric acid solution;
filtering, freeze-drying and carbonizing the cross-linked product at a preset temperature in a nitrogen atmosphere to obtain the T-Nb with the core-shell structure2O5@ C composite material.
2. Core-shell structure T-Nb according to claim 12O5The preparation method of the @ C composite material is characterized in that the mass concentration of the sodium alginate solution is 1-2%.
3. According to the rightThe core-shell structure T-Nb of claim 12O5A method for preparing a @ C composite material, characterized in that the NbCl is5The hydrochloric acid solution is prepared by adding excess NbCl5Dissolving in a hydrochloric acid solution, wherein the concentration of the hydrochloric acid solution is 0.5-1 mol/L.
4. Core-shell structure T-Nb according to claim 32O5The preparation method of the @ C composite material is characterized in that NbCl5In NbCl5The concentration of the hydrochloric acid solution is 0.05-0.15 mol/L.
5. Core-shell structure T-Nb according to claim 12O5The preparation method of the @ C composite material is characterized in that the sodium alginate solution and NbCl are mixed5The volume ratio of the hydrochloric acid solution is 3: 10-6: 10, and the hydrochloric acid solution is mixed and stirred for 24-48 hours.
6. Core-shell structure T-Nb according to claim 12O5The preparation method of the @ C composite material is characterized in that the freeze drying is carried out for 24-48h under the condition of 1Pa, -60-50 ℃.
7. Core-shell structure T-Nb according to claim 12O5The preparation method of the @ C composite material is characterized in that carbonization is carried out at high temperature under nitrogen atmosphere, the carbonization temperature is 600-700 ℃, the temperature rise rate is 5-10 ℃/min, the heat preservation time is 2-3 h, and the nitrogen flow rate is 0.6-0.8L/min.
8. Core-shell structure T-Nb prepared by the method of claim 12O5The application of the @ C composite material in the application of the anode material of the lithium ion battery with the rapid charge and discharge performance.
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