CN111933933A - Novel lithium ion battery cathode material and preparation method thereof - Google Patents
Novel lithium ion battery cathode material and preparation method thereof Download PDFInfo
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- 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
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- 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
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Abstract
The invention discloses a novel lithium ion battery cathode material and a preparation method thereof, and the design idea is as follows: s-doped ZIF-67 is synthesized by adopting a one-step method, and then the S-doped ZIF-67 and graphene oxide powder are carbonized together under inert gas to form a nano polyhedral composite material with a carbon skeleton protective layer on the outer layer based on the ZIF-67, and the nano polyhedral composite material is used for a lithium ion battery cathode. The method has simple steps, does not need expensive reaction instruments, and the prepared lithium ion battery has high energy density, good cycle performance and excellent electrochemical performance.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a novel lithium ion battery cathode material and a preparation method thereof.
Background
The lithium ion battery has the advantages of high energy density, high working voltage, long cycle life, safety and no pollution, and is one of the most concerned high-performance storage batteries, and is widely applied to portable electronic products. The current commercial lithium ion battery cathode materials are mainly artificial graphite and natural graphite materials. The theoretical specific capacity of the graphite material is only 372mAh g-1And thus cannot meet the increasing energy density requirements of lithium ion batteries. The discovery of a new generation of high-performance cathode material of lithium ion batteries is inevitable.
Metal-organic frameworks (MOFs) are a class of organic-inorganic hybrid materials that are constructed from organic ligands and inorganic Metal units. Generally having a variable topology and physicochemical properties. MOFs have wide application in the fields of gas adsorption, drug sustained release, luminescence and catalysis. The regulation and control of the catalytic performance of the catalyst is a very popular research direction at present, and has an important promoting effect on the development of catalytic chemistry.
ZIF-67 is a typical metal-organic framework material. The typical preparation method is ZIF 67: mixing the aqueous solution of cobalt nitrate hexahydrate and the aqueous solution of dimethyl imidazole. Around ZIF-67, many researchers have improved it and used it in electrodes for various electrochemical reactions. For example, Chinese patent application CN110797206A discloses a Co-Mn-S composite material and a preparation method thereof, and the Co-Mn-S composite material can be applied to a super capacitor and can reach 2397F g-1The specific capacitance of (c). Chinese patent CN108374179B discloses a preparation method of an iron-doped cobalt diselenide composite carbon-doped carbon material, and the iron-doped cobalt diselenide composite carbon-doped carbon material is used for industrial application of electrochemically decomposing water to produce hydrogen, and has the advantages of low hydrogen production overpotential, low hydrogen production Tafel slope and the like. Although the ZIF-67 is improved and has good technical effect in the prior art, the ZIF-67 is applied to the field of lithium ion battery cathodes less, and has the defects of more improvement steps, complex operation, high cost of equipment such as a hydrothermal reactor and the like, and toxic substances such as thioacetamide (2B carcinogenic substance) and the like.
Disclosure of Invention
The invention is based on ZIF-67 and aims to explore a novel lithium ion battery cathode material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the novel lithium ion battery cathode material comprises the following steps
The method comprises the following steps: dissolving a cobalt salt in a solvent to form a solution A; co-dissolving 2-methylimidazole and a sulfur source in a solvent to form a solution B;
step two: slowly dripping the solution A into the solution B under the stirring condition to form a mixed solution C, and continuously stirring for 0.5-10 h; standing for 1-48 h, centrifugally washing and drying precipitates in the mixed solution C to obtain an S-ZIF-67 precursor;
and step three, after fully mixing the S-ZIF-67 precursor with the graphene oxide powder, moving the mixture to a tubular furnace, and heating and preserving heat for 1-12 hours under the protection of inert gas, wherein the heating rate is 1-20 ℃/min, and the heat preservation temperature is 800-1200 ℃, so as to obtain the novel lithium ion battery cathode material.
As an improved technical scheme of the invention, in the first step, the cobalt salt is one of cobalt nitrate, cobalt acetate and cobalt sulfate; the sulfur source is one of thiourea and sodium thiosulfate; the solvent is water and/or alcohol, and the alcohol is one of methanol, ethanol, propanol and butanol.
As an improved technical scheme of the invention, in the first step, the concentration of the cobalt salt is 0.01-1 mol/L, the concentration of the 2-methylimidazole is 0.01-4 mol/L, and the concentration of the sulfur source is 0.01-3 mol/L.
As an improved technical scheme of the invention, in the second step, the stirring speed is 60-1000 rpm.
According to the improved technical scheme, in the third step, the mixing mode of the S-ZIF-67 precursor and the graphene oxide powder is ball milling, and the ball-powder ratio is 10-20: 1, the rotating speed is 150-250 r/min, and the ball milling time is 1-24 h.
In the third step, the inert gas is one of hydrogen, argon and nitrogen; preferably nitrogen.
As an improved technical scheme, in the third step, the mass ratio of the S-ZIF-67 precursor to the graphene oxide is 1: 0.1 to 10; preferably 1: 1 to 3.
The invention also provides a novel lithium ion battery cathode material which is prepared by adopting the method.
Has the advantages that:
the method is simple and convenient to operate, time-saving, energy-saving, efficient and good in economical efficiency. The cathode of the lithium ion battery prepared by improving the ZIF-67 has good energy density and rate capability.
The specific implementation mode is as follows:
the present invention will now be described in detail with reference to specific embodiments thereof for the purpose of clearly understanding the present invention by those skilled in the art.
Example 1
Taking 0.01mol of Co (NO)3)2·6H2Fully dissolving O into 100mL of deionized water to form solution A; then 0.04mol of 2-methylimidazole and 0.03mol of sodium thiosulfate were sufficiently co-dissolved in 100mL of deionized water to form solution B. Adjusting the stirring speed of a magnetic stirrer to be 400rpm, slowly dropwise adding the solution A into the solution B to form a solution C, continuously stirring and reacting for 2 hours, standing for 24 hours, and removing a supernatant. And repeatedly centrifuging and washing the lower-layer precipitate by using deionized water, and drying the centrifuged and washed precipitate at 70 ℃ to obtain S-doped ZIF-67, which is marked as S-ZIF-67.
Mixing S-ZIF-67 and graphene oxide powder according to a mass ratio of 1: 2, adjusting the parameters of the ball mill, wherein the ball-powder ratio is 15: 1, rotating speed is 200r/min, ball milling time is 4 hours, S-ZIF-67 and graphene oxide powder are fully mixed, then the mixture is moved into a tube furnace, nitrogen is used as protective gas, temperature rising rate is adjusted to be 10 ℃/min, heat preservation temperature is 1000 ℃, and heat preservation time is 2 hours, so that the novel lithium ion battery cathode material is prepared.
Example 2
The present embodiment is different from embodiment 1 in that: the ratio of S-ZIF-67 to graphene oxide powder is 1: 1, the rest of the same procedure as in example 1.
Example 3
The present embodiment is different from embodiment 1 in that: the ratio of S-ZIF-67 to graphene oxide powder is 1: 3, the rest of the process was the same as in example 1.
Example 4
The present embodiment is different from embodiment 1 in that: the ratio of S-ZIF-67 to graphene oxide powder is 1: 0.1, as in example 1.
Example 5
The present embodiment is different from embodiment 1 in that: the ratio of S-ZIF-67 to graphene oxide powder is 1: 10 as in example 1.
Example 6
The present embodiment is different from embodiment 1 in that: 0.01mol of Co (CH) is taken3COO)2·4H2Fully dissolving O into 100mL of ethanol to form solution A; then 0.04mol of 2-methylimidazole and 0.03mol of thiourea were sufficiently co-dissolved in 100mL of ethanol to form a solution B. Adjusting the stirring speed of a magnetic stirrer to be 400rpm, slowly dropwise adding the solution A into the solution B to form a solution C, continuously stirring and reacting for 2 hours, standing for 24 hours, and removing a supernatant. And repeatedly centrifuging and washing the lower-layer precipitate by using ethanol, and drying the centrifuged and washed precipitate at 70 ℃ to obtain S-doped ZIF-67 which is marked as S-ZIF-67. The rest is the same as example 1.
Example 7
The present embodiment is different from embodiment 1 in that: co (NO)3)2·6H2The dosage of O is 0.001mol, the dosage of 2-methylimidazole is 0.004mol, and the dosage of sodium thiosulfate is 0.003 mol. The rest is the same as example 1.
Example 8
The present embodiment is different from embodiment 1 in that: co (NO)3)2·6H2The amount of O used was 0.005mol, the amount of 2-methylimidazole used was 0.02mol, and the amount of sodium thiosulfate used was 0.015 mol. The rest is the same as example 1.
Example 9
The present embodiment is different from embodiment 1 in that: co (NO)3)2·6H2The dosage of O is 0.05mol, the dosage of 2-methylimidazole is 0.2mol, and the dosage of sodium thiosulfate is 0.15 mol. The rest is the same as example 1.
Example 10
The present embodiment is different from embodiment 1 in that: co (NO)3)2·6H2The dosage of O is 0.1mol, the dosage of 2-methylimidazole is 0.4mol, and the dosage of sodium thiosulfate is 0.3 mol. The rest is the same as example 1.
Example 11
The present embodiment is different from embodiment 1 in that: the protective gas in the tube furnace was argon. The rest is the same as example 1.
Example 12
The present embodiment is different from embodiment 1 in that: the protective gas in the tube furnace is hydrogen. The rest is the same as example 1.
Example 13
The present embodiment is different from embodiment 1 in that: the heating rate in the tube furnace is 20 ℃/min, the heat preservation temperature is 1200 ℃, and the heat preservation time is 1 h. The rest is the same as example 1.
Example 14
The present embodiment is different from embodiment 1 in that: the heating rate in the tube furnace is 1 ℃/min, the heat preservation temperature is 800 ℃, and the heat preservation time is 12 h. The rest is the same as example 1.
Example 15
The present embodiment is different from embodiment 1 in that: adjusting the parameters of the ball mill to ensure that the ball powder ratio is 10: 1, the rotating speed is 250r/min, and the ball milling time is 1 h. The rest is the same as example 1.
Example 16
The present embodiment is different from embodiment 1 in that: and (3) adjusting the parameters of the ball mill so that the ball powder ratio is 20: 1, the rotating speed is 150r/min, and the ball milling time is 24 h. The rest is the same as example 1.
Comparative example 1
Taking 0.01mol of Co (NO)3)2·6H2Fully dissolving O into 100mL of deionized water to form solution A; 0.04mol of 2-methylimidazole is then dissolved in 100mL of deionized water to form solution B. Adjusting the stirring speed of a magnetic stirrer to be 400rpm, slowly dropwise adding the solution A into the solution B to form a solution C, continuously stirring and reacting for 2 hours, standing for 24 hours, and removing a supernatant. And repeatedly centrifuging and washing the lower-layer precipitate by using deionized water, and drying the centrifuged and washed precipitate at 70 ℃ to obtain ZIF-67. The rest is the same as example 1.
Comparative example 2
S-ZIF-67 is prepared according to example 1, dried and then directly transferred to a tube furnace, the temperature rising rate is adjusted to 10 ℃/min by taking nitrogen as protective gas, the heat preservation temperature is 1000 ℃, and the heat preservation time is 2 hours. The rest is the same as example 1.
Comparative example 3
ZIF-67 was prepared according to the method of comparative example 1, then 0.03mol of sodium thiosulfate was ultrasonically dispersed with ZIF-67 in 100mL of deionized water, and then transferred to a hydrothermal reaction kettle to react at 150 ℃ for 5h to prepare sulfur-doped ZIF-67. The rest is the same as example 1.
Preparing a negative pole piece: the novel lithium ion battery negative electrode material, acetylene black and PVDF are mixed according to the mass ratio of 8: 1: 1 grinding in a mortar for more than 20min to fully mix the three. Adding a proper amount of N-methyl pyrrolidone (NMP) dropwise and stirring for 8h at room temperature under the action of a magnetic stirrer to obtain a paste material. The paste was poured onto a current collector (copper foil) uniformly and the pole piece was coated with a thickness of about 150 μm using a hand coater. Drying at 80 deg.C for 12h, and drying at 120 deg.C for 12 h. The circular pole pieces, with a diameter of about 1.2cm, were cut by a microtome and left to be assembled into button cells.
Assembling the button cell: the button cell is of a CR2016 type and is assembled in a glove box. The protective gas in the glove box is argon, and the partial pressure of water and oxygen is lower than 1 ppm. Sequentially assembling a positive electrode shell, a gasket, a lithium sheet, a diaphragm, a negative electrode sheet and a gasket which are matched with the CR2016, and dropwise adding a proper amount of electrolyte among the lithium sheet, the diaphragm and the negative electrode sheet to enable the electrolyte to fully infiltrate the diaphragm and the negative electrode sheet. And finally, sealing and compacting the assembled analog button cell under the pressure of about 4 Mpa. The assembled cell was left to stand at room temperature for 8-12 hours for testing. The charge and discharge were carried out at 0.05 to 2.5V at 0.1mA/cm2, and the results are shown in the following table.
The quality ratio of S-ZIF-67 and graphene oxide has a significant influence on the performance of the lithium ion battery. The mass ratio of the S-ZIF-67 to the graphene oxide is too large, so that the conductivity of the negative electrode material is too poor, and the electrochemical performance is poor. If the mass ratio of the S-ZIF-67 to the graphene oxide is too small, the lithium ion battery has poor electrochemical performance due to less active materials. Preferably, the mass ratio of S-ZIF-67 to graphene oxide is 1: 1 to 3. The cobalt salt concentration is too low and the yield is low. The performance of the prepared novel lithium ion battery is also deteriorated due to the overlarge concentration. Preferably, the concentration of the cobalt salt is 0.01-1 mol/L. Compared with the S-doped ZIF-67 prepared by the one-step method, the S-doped ZIF-67 prepared by the two-step method has complex preparation steps, S cannot be well doped into the ZIF-67, and the finally prepared lithium ion battery cathode material has poor cycle performance.
Variations and modifications to the above-described embodiments may occur to those skilled in the art, which fall within the scope and spirit of the above description. Therefore, the present invention is not limited to the specific embodiments disclosed and described above, and some modifications and variations of the present invention should fall within the scope of the claims of the present invention. Furthermore, although specific terms are employed herein, they are used in a generic and descriptive sense only and not for purposes of limitation.
Claims (10)
1. The preparation method of the novel lithium ion battery cathode material comprises the following steps
The method comprises the following steps: dissolving a cobalt salt in a solvent to form a solution A; co-dissolving 2-methylimidazole and a sulfur source in a solvent to form a solution B;
step two: slowly dripping the solution A into the solution B under the stirring condition to form a mixed solution C, and continuously stirring for 0.5-10 h; standing for 1-48 h, centrifugally washing and drying precipitates in the mixed solution C to obtain an S-ZIF-67 precursor;
and step three, after fully mixing the S-ZIF-67 precursor with the graphene oxide powder, moving the mixture to a tubular furnace, and heating and preserving heat for 1-12 hours under the protection of inert gas, wherein the heating rate is 1-20 ℃/min, and the heat preservation temperature is 800-1200 ℃, so as to obtain the novel lithium ion battery cathode material.
2. The preparation method of the novel lithium ion battery anode material according to claim 1, characterized in that: in the first step, the cobalt salt is one of cobalt nitrate, cobalt acetate and cobalt sulfate; the sulfur source is one of thiourea and sodium thiosulfate; the solvent is water and/or alcohol.
3. The preparation method of the novel lithium ion battery anode material according to claim 2, characterized in that: the alcohol is one of methanol, ethanol, propanol and butanol.
4. The preparation method of the novel lithium ion battery anode material according to claim 1, characterized in that: in the first step, the concentration of the cobalt salt is 0.01-1 mol/L, the concentration of the 2-methylimidazole is 0.01-4 mol/L, and the concentration of the sulfur source is 0.01-3 mol/L.
5. The preparation method of the novel lithium ion battery anode material according to claim 1, characterized in that: in the second step, the stirring speed is 60-1000 rpm.
6. The preparation method of the novel lithium ion battery anode material according to claim 1, characterized in that: in the third step, ball milling is adopted as a mixing mode of the S-ZIF-67 precursor and the graphene oxide powder, and the ball powder ratio is 10-20: 1, the rotating speed is 150-250 r/min, and the ball milling time is 1-24 h.
7. The preparation method of the novel lithium ion battery anode material according to claim 1, characterized in that: in the third step, the inert gas is one of hydrogen, argon and nitrogen.
8. The preparation method of the novel lithium ion battery anode material according to claim 1, characterized in that: in the third step, the mass ratio of the S-ZIF-67 precursor to the graphene oxide is 1: 0.1 to 10.
9. The preparation method of the novel lithium ion battery anode material according to claim 8, characterized in that: in the third step, the mass ratio of the S-ZIF-67 precursor to the graphene oxide is 1: 1 to 3.
10. A novel lithium ion battery negative electrode material prepared by the preparation method of the novel lithium ion battery negative electrode material according to any one of claims 1 to 9.
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| CN202010764821.8A CN111933933A (en) | 2020-07-31 | 2020-07-31 | Novel lithium ion battery cathode material and preparation method thereof |
| PCT/CN2020/124579 WO2022021643A1 (en) | 2020-07-31 | 2020-10-29 | Novel lithium-ion battery negative electrode material and preparation method therefor |
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Cited By (2)
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| WO2022021641A1 (en) * | 2020-07-31 | 2022-02-03 | 广东凯金新能源科技股份有限公司 | Battery negative electrode material and preparation method therefor |
| CN114497513A (en) * | 2022-03-05 | 2022-05-13 | 青岛泰达华润新能源科技有限公司 | Graphene negative electrode material for lithium ion battery and preparation method thereof |
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| CN114613999B (en) * | 2022-03-16 | 2023-09-15 | 哈尔滨工业大学（威海） | Sodium ion battery anode material with hollow nano cage structure and preparation method thereof |
| CN114725353A (en) * | 2022-04-29 | 2022-07-08 | 长江师范学院 | Novel metal chalcogenide solid solution electrode material and preparation method and application thereof |
| CN114792789B (en) * | 2022-05-02 | 2024-01-26 | 大连理工大学 | Nitrogen-doped carbon-coated nickel cobalt sulfide hollow structure, preparation method and application thereof |
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| CN115155665A (en) * | 2022-07-27 | 2022-10-11 | 云南民族大学 | Preparation method of ZIF-67-Mn low-temperature water-resistant denitration catalyst |
| CN115259101B (en) * | 2022-08-04 | 2023-07-18 | 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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| WO2022021641A1 (en) * | 2020-07-31 | 2022-02-03 | 广东凯金新能源科技股份有限公司 | Battery negative electrode material and preparation method therefor |
| CN114497513A (en) * | 2022-03-05 | 2022-05-13 | 青岛泰达华润新能源科技有限公司 | Graphene negative electrode material for lithium ion battery and preparation method thereof |
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