CN106129396A - alpha-MnO 2/graphene hollow nanotube and preparation method thereof - Google Patents
alpha-MnO 2/graphene hollow nanotube and preparation method thereof Download PDFInfo
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- CN106129396A CN106129396A CN201610647250.3A CN201610647250A CN106129396A CN 106129396 A CN106129396 A CN 106129396A CN 201610647250 A CN201610647250 A CN 201610647250A CN 106129396 A CN106129396 A CN 106129396A
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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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/502—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese for non-aqueous cells
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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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
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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 relates to the technical field of electrode materials, in particular to alpha-MnO 2 The preparation method of the graphene hollow nanotube comprises the following steps: adding graphene oxide into deionized water, and then carrying out ultrasonic oscillation; adding ascorbic acid into the solution and mixing to obtain a first mixed solution; putting the mixed solution I into a water bath kettle, and keeping the temperature constant to obtain a black precipitate; washing the black precipitate with deionized water and ethanol, and dryingDrying for later use; mixing KMnO 4 Mixing the aqueous solution with HCl to obtain a second mixed solution; adding the black precipitate into the second mixed solution, stirring and transferring into a high-pressure reaction kettle; after the reaction, cooling, washing the product with distilled water, then absolute ethyl alcohol, and finally drying to obtain alpha-MnO 2 A graphene hollow nanotube; the invention adopts a hydrothermal method to synthesize alpha-MnO 2 Graphene hollow nanotube, nanostructured MnO 2 The diffusion distance of lithium ions in the electrode material is shortened, thereby accelerating the electrochemical reaction.
Description
Technical Field
The invention relates to the technical field of electrode materials, in particular to alpha-MnO 2 Graphene hollow nanotubes and a preparation method thereof.
Background
MnO 2 Is an important transition metal oxide, and has been widely applied to lithium ion batteries, supercapacitors, zinc-manganese batteries and Li/MnO due to excellent electrochemical performance 2 The electrode active material is used in batteries such as batteries. Manganese dioxide as the negative electrode material of the lithium ion battery has the following advantages:
(1) Has higher theoretical specific capacity (1232 mAh/g). The capacity is far higher than the theoretical specific capacity (372 mAh/g) of the current commercial carbon material, and is also better than the theoretical specific capacity of other transition metal oxides. The higher theoretical specific capacity provides possibility for developing a large-capacity lithium battery negative electrode material;
(2)MnO 2 has a lower discharge plateau (about 0.40V) which is significantly lower than that of other transition metal oxide cathode materials. As a negative electrode material, a lower discharge plateau will help to increase the overall voltage and power of the battery;
(3)MnO 2 the electrode material has various crystal structures (such as alpha phase, beta phase and gamma phase, etc.), and the assembling mode of the units of the various crystal structures is favorable for understanding the relation between the structure and the performance of the electrode material;
(4)MnO 2 also has the characteristics of abundant natural reserves, low price, less environmental pollution and the like, which all lead to MnO 2 Has great potential in the application of the lithium ion battery cathode material.
However, as an electrode material, mnO 2 There are also some considerable disadvantages:
①Li + during de-intercalation, mnO 2 The volume of (a) is greatly expanded, and the crystal structure is deformed, so that the capacity is rapidly declined;
②MnO 2 intrinsic electronic conductivity (10) -5 ～10 -6 S/cm) is low, and thus electrochemical performance is poor at high rates.
Disclosure of Invention
In order to solve the above problems in the prior art, the present invention provides an α -MnO 2 Graphene hollow nanotubes and a preparation method thereof.
alpha-MnO 2 The preparation method of the graphene hollow nanotube comprises the following steps:
step one, adding graphene oxide into deionized water, and then carrying out ultrasonic oscillation treatment on the obtained solution;
step two, adding ascorbic acid into the solution subjected to ultrasonic oscillation treatment in the step one, and uniformly mixing to obtain a mixed solution I;
step three, putting the mixed solution I in the step two into a water bath kettle for constant temperature to obtain a black precipitate;
step four, washing the black precipitate with deionized water and then ethanol repeatedly, and then putting the black precipitate into an oven for drying for later use;
step five, mixing KMnO 4 Uniformly mixing the aqueous solution and HCl to obtain a mixed solution II;
step six, adding the black precipitate in the step four into the mixed solution II in the step five, uniformly stirring to obtain a mixed solution III, and transferring the mixed solution III into a high-pressure reaction kettle;
seventhly, cooling after the high-pressure reaction kettle is reacted, washing the product in the high-pressure reaction kettle to be neutral by using distilled water, then washing by using absolute ethyl alcohol, and finally drying by using an oven to obtain alpha-MnO 2 Graphene hollow nanotubes.
As a further description of the present invention, in the mixed solution in the second step, the mass ratio of the ascorbic acid to the graphene oxide is 2 to 3:1.
As a further explanation of the invention, the temperature of the water bath in the third step is 90-95 ℃.
As a further illustration of the invention, in the fifth step, the concentration of HCl is 2mol/L, and the HCl is mixed with KMnO 4 The molar ratio of (a) to (b) is 1.5 to 2.5.
As a further explanation of the invention, the volume of the mixed solution III in the step six is 60-70% of the volume of the high-pressure reaction kettle.
As a further illustration of the invention, the reaction temperature of the high-pressure reaction kettle is 120-140 ℃, and the reaction time is 10-12 h.
alpha-MnO prepared according to the above preparation method 2 Graphene hollow nanotubes.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts a hydrothermal method to synthesize alpha-MnO 2 Graphene hollow nanotube, nanostructured MnO 2 The diffusion distance of lithium ions in the electrode material is shortened, thereby accelerating the electrochemical reaction.
2. The nano material has larger specific surface area, increases the contact area with the electrolyte and is beneficial to improving the rate capability of the lithium ion battery.
3. The graphene has good conductivity and can be mixed with MnO 2 The electronic conductivity of the composite electrode material can be improved by compounding, so that MnO is improved 2 The electrochemical performance of (2).
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 shows α -MnO prepared by the preparation method of the present invention 2 XRD pattern of graphene hollow nanotube.
FIG. 2 shows α -MnO prepared by the preparation method of the present invention 2 SEM image of/graphene hollow nanotube.
FIG. 3 shows α -MnO prepared by the preparation method of the present invention 2 Raman spectrum of graphene hollow nanotube.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined purposes, the following detailed description of the embodiments, structural features and effects of the present invention will be made with reference to the accompanying drawings and examples.
Example 1:
α-MnO 2 the preparation method of the graphene hollow nanotube comprises the following steps:
step one, 0.01g of graphene oxide is added into 10mL of deionized water, and the solution is subjected to ultrasonic oscillation treatment for 2 hours.
And step two, adding 0.02g of ascorbic acid into the solution obtained in the step one, and uniformly mixing.
And step three, putting the mixed solution obtained in the step two into a water bath kettle at the temperature of 95 ℃, and keeping the temperature for 6 hours to obtain a black precipitate.
And step four, washing the black precipitate with deionized water and ethanol for 3 times respectively, and then drying the black precipitate in an oven at the temperature of 80 ℃ for later use.
Step five, mixing 30mL KMnO with the concentration of 0.067mol/L 4 The aqueous solution was mixed well with 2mL of HCl 2 mol/L.
And step six, adding the black precipitate obtained in the step four into the mixed solution obtained in the step five, stirring uniformly, and transferring into a high-pressure reaction kettle, wherein the volume of the solution is controlled to be 60% of that of the reaction kettle.
Seventhly, after the reaction kettle reacts for 12 hours at the temperature of 120 ℃, cooling, washing the obtained product to be neutral by using distilled water, then washing the product for 1 time by using absolute ethyl alcohol, and finally drying the product by using an oven at the temperature of 80 ℃ to obtain alpha-MnO 2 Graphene hollow nanotubes.
Example 2:
α-MnO 2 the preparation method of the graphene hollow nanotube comprises the following steps:
the method comprises the following steps: 0.015g of graphene oxide was added to 15mL of deionized water, and the solution was sonicated for 2h.
Step two: 0.0375g of ascorbic acid was added to the solution obtained in step one and mixed well.
Step three: and (5) putting the mixed solution obtained in the step two into a water bath kettle at the temperature of 90 ℃, and keeping the temperature for 8 hours to obtain a black precipitate.
Step four: washing the black precipitate with deionized water and ethanol for 3 times, and drying in 80 deg.C oven.
Step five: 30mL of KMnO with the concentration of 0.13mol/L 4 The aqueous solution was mixed well with 3mL of HCl 2 mol/L.
Step six: and (4) adding the black precipitate obtained in the fourth step into the mixed solution obtained in the fifth step, stirring uniformly, and transferring into a high-pressure reaction kettle, wherein the volume of the solution is controlled to be 65% of that of the reaction kettle.
Step seven: after the reaction kettle reacts for 10 hours at the temperature of 140 ℃, cooling, washing the obtained product with distilled water to be neutral, then washing the product with absolute ethyl alcohol for 1 time, and finally drying the product in an oven at the temperature of 80 ℃ to obtain alpha-MnO 2 Graphene hollow nanotubes.
Example 3:
α-MnO 2 the preparation method of the graphene hollow nanotube comprises the following steps:
the method comprises the following steps: 0.005g of graphene oxide was added to 10mL of deionized water, and the solution was sonicated for 2h.
Step two: 0.015g of ascorbic acid was added to the solution obtained in step one and mixed well.
Step three: and (5) putting the mixed solution obtained in the step two into a water bath kettle at the temperature of 93 ℃, and keeping the temperature for 7 hours to obtain a black precipitate.
Step four: washing the black precipitate with deionized water and then with ethanol for 3 times respectively, and drying in an oven at 80 deg.C.
Step five: 30mL of KMnO with the concentration of 0.053mol/L 4 The aqueous solution was mixed well with 2mL of HCl 2 mol/L.
Step six: and (4) adding the black precipitate obtained in the fourth step into the mixed solution obtained in the fifth step, stirring uniformly, and transferring into a high-pressure reaction kettle, wherein the volume of the solution is controlled to be 70% of that of the reaction kettle.
Step seven: after the reaction kettle reacts for 11 hours at the temperature of 130 ℃, cooling, washing the obtained product with distilled water to be neutral, then washing the product with absolute ethyl alcohol for 1 time, and finally drying the product in an oven at the temperature of 80 ℃ to obtain alpha-MnO 2 Graphene hollow nanotubes.
As shown in FIG. 1, alpha-MnO prepared according to the present invention 2 The XRD pattern of the graphene hollow nano-tube is completely consistent with that of a standard card NO.44-0414 in a PDF database, and the crystalline phase composition of the product is shown to be alpha-MnO 2 In addition, the visible X-ray diffraction peak has sharp peak shape and high peak intensity, which indicates MnO 2 The crystal form is well developed.
As shown in FIG. 2, alpha-MnO prepared by the present invention 2 SEM image of/graphene hollow nanotube, and alpha-MnO can be seen 2 Is in a one-dimensional hollow nano structure, and the diameter of the section is 50-100 nm.
As shown in FIG. 3, alpha-MnO prepared according to the present invention 2 The Raman spectrogram of the graphene hollow nanotube shows that graphene exists in surface products of D peaks and G peaks.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (7)
1. alpha-MnO 2 The preparation method of the graphene hollow nanotube is characterized by comprising the following steps: the method comprises the following steps:
step one, adding graphene oxide into deionized water, and then carrying out ultrasonic oscillation treatment on the obtained solution;
step two, adding ascorbic acid into the solution subjected to ultrasonic oscillation treatment in the step one, and uniformly mixing to obtain a mixed solution I;
step three, putting the mixed solution I in the step two into a water bath kettle for constant temperature to obtain a black precipitate;
step four, washing the black precipitate with deionized water and then ethanol repeatedly, and then putting the black precipitate into an oven for drying for later use;
step five, mixing KMnO 4 Uniformly mixing the aqueous solution and HCl to obtain a mixed solution II;
step six, adding the black precipitate obtained in the step four into the mixed solution II obtained in the step five, uniformly stirring to obtain a mixed solution III, and transferring the mixed solution III into a high-pressure reaction kettle;
seventhly, after the high-pressure reaction kettle is reacted, cooling, washing the product in the high-pressure reaction kettle to be neutral by using distilled water, then washing by using absolute ethyl alcohol, and finally drying by using an oven to obtain alpha-MnO 2 Graphene hollow nanotubes.
2. An α -MnO according to claim 1 2 The preparation method of the graphene hollow nanotube is characterized by comprising the following steps: in the mixed solution in the second step, the mass ratio of the ascorbic acid to the graphene oxide is 2-3:1.
3. An α -MnO according to claim 1 2 The preparation method of the graphene hollow nanotube is characterized by comprising the following steps: in the third step, the temperature of the water bath kettle is 90-95 ℃.
4. An α -MnO according to claim 1 2 The preparation method of the graphene hollow nanotube is characterized by comprising the following steps: in the fifth step, the concentration of the HCl is 2mol/L, and the HCl and the KMnO are 4 The molar ratio of (a) to (b) is 1.5 to 2.5.
5. An α -MnO according to claim 1 2 The preparation method of the graphene hollow nanotube is characterized by comprising the following steps: and sixthly, the volume of the mixed solution III is 60-70% of the volume of the high-pressure reaction kettle.
6. An α -MnO according to claim 1 2 The preparation method of the graphene hollow nanotube is characterized by comprising the following steps: the reaction temperature of the high-pressure reaction kettle is 120-140 ℃, and the reaction time is 10-12 h.
7. alpha-MnO prepared by the preparation method according to any one of claims 1 to 6 2 Graphene hollow nanotubes.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109830683A (en) * | 2019-02-18 | 2019-05-31 | 山东星火科学技术研究院 | A kind of preparation method of the powerful nitrogen-doped graphene negative electrode material of high capacity |
| CN110104689A (en) * | 2019-03-27 | 2019-08-09 | 河南省人民医院 | A kind of hollow manganese dioxide nano particle and preparation method thereof |
| CN113707868A (en) * | 2021-08-31 | 2021-11-26 | 中国地质大学（北京） | Ternary composite electrode material, preparation method thereof and zinc ion battery |
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| CN102275903A (en) * | 2011-05-24 | 2011-12-14 | 东华大学 | Preparation method of graphene and manganese dioxide nanocomposite |
| CN103489660A (en) * | 2013-09-05 | 2014-01-01 | 北京工业大学 | Manganese dioxide nanorod/graphene composite electrode material and preparation method thereof |
| CN103915613A (en) * | 2014-04-10 | 2014-07-09 | 山东润昇电源科技有限公司 | Preparation method of hydro-thermal coupling spray pyrolysis MnO2/graphene electrode material |
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2016
- 2016-08-09 CN CN201610647250.3A patent/CN106129396A/en active Pending
Patent Citations (3)
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| CN102275903A (en) * | 2011-05-24 | 2011-12-14 | 东华大学 | Preparation method of graphene and manganese dioxide nanocomposite |
| CN103489660A (en) * | 2013-09-05 | 2014-01-01 | 北京工业大学 | Manganese dioxide nanorod/graphene composite electrode material and preparation method thereof |
| CN103915613A (en) * | 2014-04-10 | 2014-07-09 | 山东润昇电源科技有限公司 | Preparation method of hydro-thermal coupling spray pyrolysis MnO2/graphene electrode material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109830683A (en) * | 2019-02-18 | 2019-05-31 | 山东星火科学技术研究院 | A kind of preparation method of the powerful nitrogen-doped graphene negative electrode material of high capacity |
| CN110104689A (en) * | 2019-03-27 | 2019-08-09 | 河南省人民医院 | A kind of hollow manganese dioxide nano particle and preparation method thereof |
| CN110104689B (en) * | 2019-03-27 | 2021-08-13 | 河南省人民医院 | Hollow manganese dioxide nano-particles and preparation method thereof |
| CN113707868A (en) * | 2021-08-31 | 2021-11-26 | 中国地质大学（北京） | Ternary composite electrode material, preparation method thereof and zinc ion battery |
| CN113707868B (en) * | 2021-08-31 | 2022-10-21 | 中国地质大学（北京） | Ternary composite electrode material, preparation method thereof and zinc ion battery |
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