CN112875765B - NiMnO 3 Preparation method of bimetal oxide and energy storage device - Google Patents
NiMnO 3 Preparation method of bimetal oxide and energy storage device Download PDFInfo
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- CN112875765B CN112875765B CN202110063564.XA CN202110063564A CN112875765B CN 112875765 B CN112875765 B CN 112875765B CN 202110063564 A CN202110063564 A CN 202110063564A CN 112875765 B CN112875765 B CN 112875765B
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- C01G53/00—Compounds of nickel
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
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- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
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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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a NiMnO 3 The preparation method of the bimetal oxide and the energy storage device comprise the following steps: (1) Mixing potassium permanganate, nickel salt, ammonium chloride and a solvent to form a mixed solution, transferring the mixed solution into a closed container to react at 130-150 ℃, separating solid from liquid of the reacted product, taking solid, and drying to obtain NiMnO 3 A precursor; (2) Taking the NiMnO 3 The precursor is heated to 570-630 ℃ in an oxygen-containing atmosphere for calcination. The method of the invention has simple synthesis and convenient operation, and can prepare the NiMnO forming the hollow nanospheres by using the potassium permanganate, the nickel salt and the ammonium chloride as reaction raw materials 3 The prepared material can be applied to preparing electrode materials, and has a wide application prospect in the fields of energy storage devices such as batteries, super capacitors and the like.
Description
Technical Field
The invention relates to a preparation method of NiMnO3 bimetallic oxide and an energy storage device.
Background
The nano material has a wide application prospect in catalysis, batteries, sensing, electronic materials, optical materials, magnetic materials and the like due to various characteristics such as unique size effect, quantum effect, interface effect and the like. Two-dimensional (2D) materials play an important role in various fields from basic science to science technology due to their unique physical and electrochemical properties. The unique properties of 2D materials have attracted an increasing number of researchers looking for a variety of new 2D materials. Transition metal oxides have excellent electrochemical and catalytic properties and have been widely used in various fields of catalysis, energy conversion and storage. However, the performance of transition metal oxides has not reached the desired level in energy storage applications, and the electrochemical properties of these materials are also highly dependent on their dimensional nanostructures. In recent years, single metal oxides have been increasingly used because of their better conductivity and electrochemical propertiesResearchers have focused on developing binary and ternary transition metal oxides as electrode materials for energy storage applications. Chinese patent document CN102583586A (application number 201110008071.2) discloses an ilmenite type NiMnO 3 Is prepared by mixing NaHCO with 3 Adding the solution into a mixture of soluble nickel salt and manganese salt, precipitating, stirring, suction filtering, washing, drying and grinding to obtain a precursor (a mixture of manganese carbonate and nickel carbonate), and performing acid treatment to obtain NiMnO 3 A material. NiMnO in the invention 3 The preparation method of (2) is complex, which prolongs the production time and increases the production cost.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. To this end, the invention proposes a NiMnO 3 The preparation method of the bimetallic oxide has simple synthesis and convenient operation, and is beneficial to mass production of NiMnO 3 Bimetallic oxide, niMnO prepared therefrom 3 The bimetal oxide has a hollow nanosphere structure, can be applied to the preparation of electrode materials, and can be applied to the fields of energy storage devices such as batteries, supercapacitors and the like.
In a first aspect of the present invention, there is provided a method for preparing a NiMnO3 bimetallic oxide comprising the steps of:
(1) Mixing potassium permanganate, nickel salt, ammonium chloride and a solvent to form a mixed solution, transferring the mixed solution into a closed container to react at 130-150 ℃, separating solid from liquid of the reacted product, taking solid, and drying to obtain NiMnO 3 A precursor;
(2) Taking the NiMnO 3 The precursor is heated to 570-630 ℃ in an oxygen-containing atmosphere for calcination.
NiMnO according to an embodiment of the present invention 3 The preparation method of the bimetallic oxide has at least the following beneficial effects:
the embodiment of the invention provides a NiMnO 3 The preparation method of the bimetallic oxide uses potassium permanganate, nickel salt and ammonium chloride as reaction raw materials for preparation, urea is not needed for adjusting pH, and the ammonium chloride is used in comparison with ammonium fluorideHas better stability, is not easy to hydrolyze in solution, and is favorable for the subsequent formation of hollow micro-nano sphere structures. The preparation method provided by the embodiment of the invention has the advantages of simple synthesis and convenient operation, and is beneficial to mass production of NiMnO 3 Bimetallic oxide, niMnO prepared by the preparation method of the embodiment of the invention 3 The bimetal oxide has uniform size and complete morphology, can be applied to preparing electrode materials, and has a great application prospect in the fields of energy storage devices such as batteries, super capacitors and the like.
NiMnO according to an embodiment of the present invention 3 A preparation method of a bimetallic oxide, wherein the potassium permanganate comprises the following steps: nickel salt: the molar ratio of the ammonium chloride is 1:1: (0.8-1.2). Although both ammonium chloride and ammonium fluoride are ionic compounds, fluoride ions are more basic than chloride ions, and ammonium fluoride tends to be decomposed into ammonia gas and hydrogen halide than ammonium chloride, so that when both are in solution, fluoride ions are hydrolyzed, chloride ions are not, and ammonium chloride is relatively stable. The embodiment of the invention uses ammonium chloride with stronger stability, combines potassium permanganate and nickel salt, adjusts the reaction proportion of raw materials and leads the finally prepared NiMnO 3 The bimetallic oxide has good surface morphology.
NiMnO according to an embodiment of the present invention 3 The preparation method of the bimetallic oxide comprises the step of preparing water as the solvent. In the prior art, niMnO is prepared 3 When the material is dissolved in ethylene glycol for hydrothermal reaction, but the ethylene glycol is toxic, if the material is produced in a large amount in industry, certain harm can be caused to human bodies, and the raw materials used in the embodiment of the invention can be used for hydrothermal reaction by using green water as a solvent, so that the cost is low and the environment is protected.
NiMnO according to an embodiment of the present invention 3 The preparation method of the bimetal oxide comprises the step of providing a nickel source, wherein the nickel salt is nickel nitrate or nickel sulfate.
NiMnO according to an embodiment of the present invention 3 In the preparation method of the bimetallic oxide, in the step (2), the calcination time is 2-4 h.
NiMnO according to an embodiment of the present invention 3 Method for producing a bimetallic oxide, wherein in step (2), the temperature is raisedThe temperature rate is 2-4 ℃/min. If the temperature rising rate is high, the structure and the morphology of the prepared substance are possibly incomplete, and the performance of the material is affected.
NiMnO according to an embodiment of the present invention 3 In the preparation method of the bimetallic oxide, in the step (1), the reaction time is 20-48 hours.
The oxygen-containing atmosphere in this application means that the atmosphere contains oxygen. NiMnO according to an embodiment of the present invention 3 In the preparation method of the bimetallic oxide, in the step (2), the oxygen-containing atmosphere is an air atmosphere.
NiMnO according to an embodiment of the present invention 3 The preparation method of the bimetallic oxide, in the step (1), further comprises a process of washing the solid before the step of drying.
NiMnO according to an embodiment of the present invention 3 In the preparation method of the bimetallic oxide, in the step (1), water and/or absolute ethyl alcohol are used for washing the solid. Further preferably, in step (1), the solid is washed sequentially with water and absolute ethanol before the drying step.
NiMnO according to an embodiment of the present invention 3 The preparation process of bimetal oxide with drying temperature of 50-80 deg.c.
In a second aspect of the invention, there is provided a NiMnO 3 Bimetallic oxides, according to NiMnO described above 3 The preparation method of the bimetallic oxide.
In a third aspect of the present invention, there is provided an electrode material comprising the above NiMnO 3 A bimetallic oxide.
In a fourth aspect of the present invention, an energy storage device is provided, comprising the electrode material described above.
According to some embodiments of the invention, the energy storage device is a battery or a supercapacitor.
Drawings
The invention is further described with reference to the accompanying drawings and examples, in which:
FIG. 1 shows NiMnO obtained in example 1 of the present invention 3 XRD pattern of the bimetallic oxide;
FIG. 2 is a view of NiMnO obtained in example 1 of the present invention 3 SEM images of the precursor;
FIG. 3 shows NiMnO obtained in example 1 of the present invention 3 Electron microscope pictures of the bimetallic oxide;
FIG. 4 shows the NiMnO obtained after calcination at 650℃in comparative example 1 3 SEM images of the bimetallic oxide at different magnifications under scanning electron microscope.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
Example 1
The present embodiment provides a NiMnO 3 A bimetallic oxide prepared according to the steps of:
(1) 0.316g of potassium permanganate (KMnO) was weighed out 4 ) Dissolved in 160mL of deionized water, stirred on a magnetic stirrer, and 0.58g of nickel nitrate (Ni (NO) was added, respectively 3 )·6H 2 O) and 0.107g of ammonium chloride (NH) 4 Cl) was mixed and stirred in the solution until uniform. Transferring the stirred solution into a reaction kettle, transferring the reaction kettle into a reaction oven, performing hydrothermal reaction for 24 hours at 140 ℃, filtering and washing with deionized water, washing with absolute ethyl alcohol, and performing forced air drying at 60 ℃ to prepare NiMnO 3 A precursor.
(2) NiMnO is added to 3 The precursor is put into a tube furnace, and is heated to 600 ℃ in air at the speed of 3 ℃/min for calcination for 3 hours, thus obtaining NiMnO 3 A bimetallic oxide.
FIG. 1 shows NiMnO obtained in this example 3 As can be seen from the figure, the XRD pattern of the bimetallic oxide can be seen, and the NiMnO can be successfully prepared by the preparation method 3 A bimetallic oxide.
FIG. 2 shows NiMnO in the present embodiment 3 FIG. 3 is an SEM image of a precursor, and FIG. 3 shows NiMnO obtained in this example 3 Electron microscopy pictures of bimetallic oxide, wherein (a) and (b) respectively represent SEM pictures of different magnifications under a scanning electron microscope, and (c) and (d) respectively represent TEM pictures of different magnifications under a transmission electron microscope. As can be seen from the figure, niMnO 3 After the precursor is heated and calcined, the ultrathin nanosheets self-assemble to form the NiMnO of the hollow nanospheres 3 The bimetal oxide material has uniform size and complete appearance, and the unique structure is favorable for being applied to the energy storage fields of batteries, supercapacitors and the like.
Effect comparative example
Comparative example 1: comparative example 1 provides a NiMnO 3 A bimetallic oxide prepared according to the steps of:
(1) 0.316g of potassium permanganate (KMnO) was weighed out 4 ) Dissolved in 160mL of deionized water, stirred on a magnetic stirrer, and 0.58g of nickel nitrate (Ni (NO) was added, respectively 3 )·6H 2 O) and 0.107g of ammonium chloride (NH) 4 Cl) was mixed and stirred in the solution until uniform. Transferring the stirred solution into a reaction kettle, transferring to a reaction oven, performing hydrothermal reaction for 24 hours at 140 ℃, filtering and washing with deionized water, washing with absolute ethyl alcohol, and performing forced air drying at 60 ℃ to prepare NiMnO 3 A precursor.
(2) Placing the precursor into a tube furnace, heating to 650 ℃ in air at a speed of 3 ℃/min for calcination for 3 hours to obtain NiMnO 3 A bimetallic oxide.
FIG. 4 shows the NiMnO obtained after calcination at 650℃in comparative example 1 3 SEM pictures of bimetallic oxide, (a) and (b) show SEM pictures of different magnifications under a scanning electron microscope respectively, and NiMnO obtained by calcination treatment at 600℃in example 1 3 The morphology comparison of the bimetallic oxide shows that the morphology of the material calcined at 600 ℃ in the embodiment 1 is better, and the ultrathin nanosheetsCan self-assemble to form hollow micro-nano spheres, but the flaky morphology of the comparative example 1 is completely absent after being calcined at 650 ℃, and all the particles are converted into particles. Experimental results show that unique hollow nanosphere structures cannot be formed when the calcination temperature reaches above 650 ℃.
Example 2
The present embodiment provides a NiMnO 3 A bimetallic oxide prepared according to the steps of:
(1) 0.316g of potassium permanganate (KMnO) was weighed out 4 ) Dissolved in 160mL of deionized water, stirred on a magnetic stirrer, and 0.58g of nickel nitrate (Ni (NO) was added, respectively 3 )·6H 2 O) and 0.086g of ammonium chloride (NH) 4 Cl) was mixed and stirred in the solution until uniform. Transferring the stirred solution into a reaction kettle, transferring the reaction kettle into a reaction oven, performing hydrothermal reaction at 130 ℃ for 40 hours, filtering and washing with deionized water, washing with absolute ethyl alcohol, and performing forced air drying at 50 ℃ to prepare NiMnO 3 A precursor.
(2) NiMnO is added to 3 The precursor is put into a tube furnace, and is heated to 630 ℃ in oxygen at the speed of 4 ℃/min for calcination, and the calcination time is 4 hours, thus obtaining NiMnO 3 A bimetallic oxide.
Taking NiMnO prepared in the embodiment 3 The bi-metal oxide was characterized and its SEM image showed a hollow nanosphere structure like that in fig. 2, the unique structure of which was such that the NiMnO in either the cell or supercapacitor 3 The bimetallic oxide material has great application potential.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.
Claims (9)
1. NiMnO 3 The preparation method of the bimetallic oxide is characterized by comprising the following steps:
(1) Mixing potassium permanganate, nickel salt, ammonium chloride and a solvent to form a mixed solution, transferring the mixed solution into a closed container, reacting for 20-48 h at 130-150 ℃, separating solid from liquid of the reacted product, taking solid, and drying to obtain NiMnO 3 A precursor; the potassium permanganate: nickel salt: the molar ratio of the ammonium chloride is 1:1: (0.8-1.2);
(2) Taking the NiMnO 3 And heating the precursor to 570-630 ℃ in an oxygen-containing atmosphere, and calcining.
2. The NiMnO of claim 1 3 The preparation method of the bimetallic oxide is characterized in that in the step (2), the calcination time is 2-4 hours.
3. The NiMnO of claim 1 3 The preparation method of the bimetal oxide is characterized in that in the step (2), the heating rate of heating is 2-4 ℃/min.
4. A NiMnO according to any one of claims 1 to 3 3 The preparation method of the bimetallic oxide is characterized in that in the step (2), the oxygen-containing atmosphere is an air atmosphere.
5. A NiMnO according to any one of claims 1 to 3 3 The preparation method of the bimetallic oxide is characterized in that in the step (1), a process of washing the solid is further included before the step of drying.
6. The method for producing NiMnO3 bimetallic oxide as claimed in claim 5, wherein the solid is washed with water and/or absolute ethanol.
7. NiMnO 3 Bimetallic oxide, characterized by NiMnO according to any one of claims 1 to 6 3 The preparation method of the bimetallic oxide.
8. An electrode material comprising the NiMnO of claim 7 3 A bimetallic oxide.
9. An energy storage device comprising the electrode material of claim 8.
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