CN111453774A - Preparation method, product and application of zinc ferrite nano flower-shaped negative electrode material - Google Patents
Preparation method, product and application of zinc ferrite nano flower-shaped negative electrode material Download PDFInfo
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- CN111453774A CN111453774A CN202010282848.3A CN202010282848A CN111453774A CN 111453774 A CN111453774 A CN 111453774A CN 202010282848 A CN202010282848 A CN 202010282848A CN 111453774 A CN111453774 A CN 111453774A
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- 229910001308 Zinc ferrite Inorganic materials 0.000 title claims abstract description 24
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000007773 negative electrode material Substances 0.000 title claims description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 7
- 239000011701 zinc Substances 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 30
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 11
- 229910001416 lithium ion Inorganic materials 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 10
- UMPKMCDVBZFQOK-UHFFFAOYSA-N potassium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[K+].[Fe+3] UMPKMCDVBZFQOK-UHFFFAOYSA-N 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims description 4
- 150000003751 zinc Chemical class 0.000 claims description 4
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 3
- 239000010406 cathode material Substances 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002057 nanoflower Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
-
- 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
- H01M4/36—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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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 provides a preparation method of a zinc ferrite nanometer flower-shaped cathode material, which utilizes redox precipitation reaction to realize solid-liquid separation, and then utilizes a method of combining liquid phase acid radical and zinc source hydrothermal reaction to prepare nanometer flower-shaped zinc ferrite. The first discharge specific capacity is 1240mAh/g under the current density of 800mA/g, the discharge specific capacity is relatively stable after 10 cycles and is 497mAh/g, and the discharge specific capacity is 394mAh/g after 50 cycles. The preparation process is relatively simple, the reaction is thorough, and the operation is easy.
Description
Technical Field
The invention relates to a preparation method of a lithium battery negative electrode material, in particular to a preparation method of a zinc ferrite nano flower-shaped negative electrode material, and a product and application thereof.
Background
With the development of society, lithium ion batteries are receiving much attention. The lithium ion battery is the most ideal rechargeable battery in the world at present, and has the advantages of high energy density, long cycle life, no memory effect, small pollution and the like. With the progress of technology, lithium ion batteries are widely applied to the fields of electric automobiles, aerospace, biomedicine and the like, so that the research and development of lithium ion batteries for power and related materials have great significance. For power lithium ion batteries, the key is to increase the power density and energy density, and the improvement of the power density and energy density is fundamentally the improvement of electrode materials, particularly negative electrode materials.
Since the early 90 s of the last century, the japanese scientists developed carbon materials with layered structures, which were the first materials studied by people and applied to the commercialization of lithium ion batteries, and still remain one of the major points of attention and research, but carbon negative electrode materials have some defects: when the battery is formed, the electrolyte reacts with the electrolyte to form an SEI film, so that the electrolyte is consumed and the first coulombic efficiency is low; when the battery is overcharged, metal lithium may be precipitated on the surface of the carbon electrode to form lithium dendrite to cause short circuit, so that the temperature is increased and the battery explodes; in addition, the diffusion coefficient of lithium ions in the carbon material is small, so that the battery cannot realize large-current charging and discharging, and the application range of the lithium ion battery is limited.
Zinc ferrite is a spinel-structured composite oxide, can be used as a lithium ion battery cathode material at present, and has higher L i + storage capacity through conversion and alloying reactions.
Disclosure of Invention
In order to overcome the defect of poor electrochemical performance caused by agglomeration or pulverization of zinc ferrite in the charging and discharging processes, the invention aims to: a method for preparing a zinc ferrite nano flower-shaped negative electrode material.
Yet another object of the present invention is to: there is provided a product obtained by the above process.
Yet another object of the present invention is to: provides an application of the product.
The invention relates to a preparation method of a zinc ferrite nano flower-shaped negative electrode material, which is characterized by comprising the following specific steps:
(1) dissolving 2.942g of potassium dichromate in deionized water, and continuously magnetically stirring until the potassium dichromate is completely dissolved to form a solution A; then weighing 0.8g of iron oxide powder, adding a small amount of deionized water, and magnetically stirring for 30 min; dropwise adding the solution A into an iron oxide aqueous solution, centrifuging after the reaction is completed, and reserving a potassium ferrite reaction liquid which is marked as a solution B, wherein the molar weight ratio of potassium dichromate to iron oxide is 2: 1;
(2) adding 0.2-0.4 g of polyvinylpyrrolidone (PVP), 10-15 m of L strong acid and a certain amount of soluble zinc salt into a potassium ferrite solution, wherein the molar ratio of iron to zinc is 1:1, magnetically stirring for 0.5-1 h, transferring into a hydrothermal reaction kettle, reacting at 160-180 ℃ for 12-16 h, naturally cooling, centrifuging the obtained product, washing with deionized water and ethanol for 2-3 times respectively, and finally drying at 60-80 ℃ overnight in vacuum to obtain the final product.
The strong acid is one or the combination of hydrochloric acid or nitric acid.
The zinc salt is one or the combination of zinc nitrate hexahydrate and zinc acetate dihydrate.
The invention provides a zinc ferrite nano flower-shaped negative electrode material which is characterized by being prepared according to any one of the methods.
The invention provides an application of a zinc ferrite nanometer flower-shaped negative electrode material as a negative electrode material of a lithium ion battery.
Has the advantages that:
the invention provides a preparation method of a zinc ferrite nanometer flower-shaped cathode material, which utilizes redox precipitation reaction to realize solid-liquid separation, and then utilizes a method of combining liquid phase acid radical and zinc source hydrothermal reaction to prepare nanometer flower-shaped zinc ferrite. The preparation process is relatively simple, the reaction is thorough, and the operation is easy.
Drawings
FIG. 1 is a cycle life diagram of a zinc ferrite nanoflower-shaped anode material of example 1;
FIG. 2 is a graph showing the cycle life of the zinc ferrite nano flower-like negative electrode material of example 2;
FIG. 3 is a graph showing the first charge and discharge performance of the zinc ferrite nano flower-like negative electrode material of example 3.
Detailed Description
The present invention is described in detail by the following specific examples, but the scope of the present invention is not limited to these examples.
The first embodiment is as follows:
dissolving 2.942g of potassium dichromate in deionized water, continuously magnetically stirring until the potassium dichromate is completely dissolved to form a solution A, then weighing 0.8g of iron oxide powder, adding a small amount of deionized water, magnetically stirring for 30min, dropwise adding the solution A into the iron oxide aqueous solution, centrifuging after the reaction is complete, reserving potassium ferrite reaction liquid, marking as a solution B, wherein the molar ratio of potassium dichromate to iron oxide is 2:1, adding 0.2g of polyvinylpyrrolidone (PVP), 10m L hydrochloric acid and 1.098g of zinc acetate dihydrate into the potassium ferrite solution, wherein the molar ratio of iron to zinc is 1:1, magnetically stirring for 0.5h, transferring into a hydrothermal reaction kettle, reacting for 16h at 160 ℃, naturally cooling, centrifuging the obtained product, washing for 3 times with deionized water and ethanol, finally drying in vacuum overnight at 60 ℃ to obtain a final product, wherein the zinc ferrite nanoflower electrode material has a cycle life chart under 800 mAh/g current density, a first discharge capacity of 1240 h, a specific discharge capacity of 1240 g/g, a specific discharge capacity of 10 mAh and a specific discharge capacity of 497/g after 50 h of specific discharge.
Example two:
dissolving 2.942g of potassium dichromate in deionized water, continuously magnetically stirring until the potassium dichromate is completely dissolved to form a solution A, then weighing 0.8g of iron oxide powder, adding a small amount of deionized water, magnetically stirring for 30min, dropwise adding the solution A into the iron oxide aqueous solution, centrifuging after the reaction is complete, reserving potassium ferrite reaction liquid, marking as a solution B, wherein the molar ratio of potassium dichromate to iron oxide is 2:1, adding 0.4g of polyvinylpyrrolidone (PVP), 15m L nitric acid and 1.098g of zinc acetate dihydrate into the potassium ferrite solution, wherein the molar ratio of iron to zinc is 1:1, magnetically stirring for 1h, transferring into a hydrothermal reaction kettle, reacting for 12h at 180 ℃, naturally cooling, centrifuging the obtained product, washing for 3 times with deionized water and ethanol, finally drying in vacuum at 80 ℃ overnight, and obtaining a final product, wherein FIG. 2 is a cycle life diagram of the zinc ferrite nano flower-shaped negative electrode material under 800mA/g current density, the first discharge capacity is 1200mAh/g, the specific discharge capacity is more than 10 mAh, and the specific discharge capacity is more stable than 400 mAh/246 after the specific discharge capacity is 400 mAh.
Example three:
dissolving 2.942g of potassium dichromate in deionized water, continuously magnetically stirring until the potassium dichromate is completely dissolved to form a solution A, then weighing 0.8g of iron oxide powder, adding a small amount of deionized water, magnetically stirring for 30min, dropwise adding the solution A into the iron oxide aqueous solution, centrifuging after the reaction is complete, reserving a potassium ferrite reaction liquid, marking as a solution B, wherein the molar ratio of potassium dichromate to iron oxide is 2:1, adding 0.4g of polyvinylpyrrolidone (PVP), 15m L nitric acid and 1.487g of zinc nitrate hexahydrate into the potassium ferrite solution, wherein the molar ratio of iron to zinc is 1:1, magnetically stirring for 1h, transferring into a hydrothermal reaction kettle, reacting for 12h at 180 ℃, naturally cooling, centrifuging the obtained product, washing for 3 times with deionized water and ethanol, and finally drying in vacuum overnight at 80 ℃ to obtain a final product, wherein the final product is shown in a graph of the first charge-discharge performance of the zinc ferrite nano flower-like negative electrode material under 800mA/g current density, the first discharge specific capacity is 158h/g, and the first charge capacity is 816 mAmAh/g.
Claims (5)
1. The invention relates to a preparation method of a zinc ferrite nano flower-shaped negative electrode material, which is characterized by comprising the following specific steps:
(1) dissolving 2.942g of potassium dichromate in deionized water, and continuously magnetically stirring until the potassium dichromate is completely dissolved to form a solution A; then weighing 0.8g of iron oxide powder, adding a small amount of deionized water, and magnetically stirring for 30 min; dropwise adding the solution A into an iron oxide aqueous solution, centrifuging after the reaction is completed, and reserving a potassium ferrite reaction liquid which is marked as a solution B, wherein the molar weight ratio of potassium dichromate to iron oxide is 2: 1;
(2) adding 0.2-0.4 g of polyvinylpyrrolidone (PVP), 10-15 m of L strong acid and a certain amount of soluble zinc salt into a potassium ferrite solution, wherein the molar ratio of iron to zinc is 1:1, magnetically stirring for 0.5-1 h, transferring into a hydrothermal reaction kettle, reacting at 160-180 ℃ for 12-16 h, naturally cooling, centrifuging the obtained product, washing with deionized water and ethanol for 2-3 times respectively, and finally drying at 60-80 ℃ overnight in vacuum to obtain the final product.
2. The method for preparing the zinc ferrite nano flower-shaped negative electrode material according to claim 1, wherein the strong acid is one or a combination of hydrochloric acid and nitric acid.
3. The method for preparing the zinc ferrite nano flower-shaped negative electrode material according to claim 1, wherein the zinc salt is one or a combination of zinc nitrate hexahydrate and zinc acetate dihydrate.
4. A zinc ferrite nano flower-like negative electrode material characterized by being prepared according to the method of any one of claims 1 to 3.
5. The application of the zinc ferrite nano flower-shaped negative electrode material as the negative electrode material of the lithium ion battery according to claim 4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115259101A (en) * | 2022-08-04 | 2022-11-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of three-dimensional core-shell hollow magnesium sulfide nanoflower |
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Application publication date: 20200728 |