LU601996B1 - Method of preparing an amorphous moo2-x@c composite material - Google Patents

Method of preparing an amorphous moo2-x@c composite material

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Publication number
LU601996B1
LU601996B1 LU601996A LU601996A LU601996B1 LU 601996 B1 LU601996 B1 LU 601996B1 LU 601996 A LU601996 A LU 601996A LU 601996 A LU601996 A LU 601996A LU 601996 B1 LU601996 B1 LU 601996B1
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amorphous
composite material
ethanol
preparing
precursor
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LU601996A
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German (de)
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Zhenjiang Lu
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Univ Xinjiang
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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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/02—Oxides; Hydroxides
    • 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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The present invention relates to the technical field of amorphous preparation technology, in particular to a method of preparing an amorphous MoO2-x@C composite material, including the following steps. S1: dissolving phosphomolybdic acid in ethanol to prepare a phosphomolybdic acid ethanol solution; subsequently, dissolving 2- methylimidazole in another portion of ethanol to form a 2-methylimidazole ethanol solution and then adding to the phosphomolybdic acid ethanol solution; then, allowing the mixed solution to stand, and collecting the resulting Mo-MI precursor by centrifugation; S2: dispersing the Mo-MI precursor (formed by the reaction of phosphomolybdic acid and 2-methylimidazole) nanospheres obtained in step S1 in deionized water, followed by stirring; then, dropwise adding a pyrrole solution and continuously stirring in an ice-water bath; subsequently, performing centrifugation to obtain a polypyrrole-coated Mo-MI (Mo- MI@PPy) precursor. Fig.1

Description

DESCRIPTION LU601996
METHOD OF PREPARING AN AMORPHOUS MOOz.x@C COMPOSITE
MATERIAL
TECHNICAL FIELD
The present invention relates to the technical field of amorphous preparation technology, and in particular to a method of preparing an amorphous MoO>,@C composite material.
BACKGROUND
MoO», due to its unique distorted rutile crystal structure, is conducive to the intercalation and deintercalation of Li+ in the material, showing the high capacity reversibility and thus possessing great potential for industrial applications. However, limited by current preparation methods, lower electrical conductivity, and volume expansion during cycling process, MoO: faces the challenges of poor cycling performance and poor cycling stability when used as an electrode material, which together restrict the process of its large-scale application.
An existing Chinese patent document CN201911410269.6 discloses a method for synthesizing MoO-@C nanofiber flexible thin-film material by electrospinning technology.
The steps of the method for synthesizing MoO:@C nanofiber flexible film material by electrostatic spinning technology according to this invention are as follows: dissolving a molybdenum source in a mixture of deionized water and ethylene glycol to obtain a solution A; adding polyvinylpyrrolidone (PVP) to the solution A and dissolving the mixture to obtain solution B; and solution B is subjected to electrospinning, drying, pre-oxidation, and sintering under an inert atmosphere to obtain the MoO.@C nanofiber flexible thin- film material.
An existing Chinese patent document CN201210100507.5 discloses a method of preparing a molybdenum dioxide/carbon composite anode material, including the following steps: 1) soaking a cotton fiber fabric of a certain size in an ethanol solution of phosphomolybdic acid and stirring; 2) drying and aging the soaked cotton fiber fabric; 3) performing a heat treatment to the dried and aged cotton fiber fabric in a mixed atmosphere to obtain a molybdenum dioxide/carbon (MoQO2/C) composite material.
The above preparation methods all have the disadvantages of complicated preparation process, many influencing factors, poor reproducibility, etc, and the prepared 0 electrode materials are ineffective and highly prone to waste of resources. In addition, the above problems only consider accelerating the diffusion of Li* in porous channels and at the solid/liquid interfaces, but cannot promote the rapid migration of Li* in the MoO: crystal structure.
SUMMARY
The objective of the present invention is to provide a method of preparing an amorphous MoO2.x@C composite material, the method of the present invention obtains amorphous MoO2.x@C by rapid annealing at low temperature. The amorphous nature significantly enhances its electronic conductivity and optimizes the migration pattern of
Li*, which greatly improves the rate performance of the material. More importantly, the combination of this amorphous structure and the carbon coating layer provides the necessary volume expansion buffer space for MoO» during the charge and discharge cycling, which effectively enhances its lithium storage capacity and cycling stability and prolongs its cycle life.
To achieve the above technical objectives and achieve the above technical effects, the present invention is achieved through the following technical schemes.
A method of preparing an amorphous MoOz,@C composite material, using phosphomolybdic acid as a molybdenum source and pyrrole as a carbon source, including the following steps.
S1: dissolving phosphomolybdic acid in ethanol to prepare a phosphomolybdic acid ethanol solution; subsequently, dissolving 2-methylimidazole in another portion of ethanol to form a 2-methylimidazole ethanol solution and then adding to the phosphomolybdic acid ethanol solution; then, allowing the mixed solution to stand, and collecting the resulting Mo-MI precursor by centrifugation.
S2: dispersing the Mo-MI precursor (formed by the reaction of phosphomolybdic acid and 2- methylimidazole) nanospheres obtained in step S1 in deionized water, followed by stirring; then, dropwise adding a pyrrole solution and continuously stirring in an ice-water bath; subsequently, performing centrifugation to obtain a polypyrrole-coated Mo-MI (Mo-
MI@PPYy) precursor, followed by vacuum-drying the precursor at 60°C for 24 hours.
S3: subjecting the dried Mo-MI@PPy precursor to pyrolysis at 450°C for 2 hours under a nitrogen atmosphere, thereby obtaining an amorphous MoO>,@C composite "996 material (0 <x < 1).
Further, in S1, a ratio of phosphomolybdic acid to ethanol is 0.06 mmol: 100 mL.
Further, in S1, a ratio of 2-methylimidazole to ethanol is 12.0 mml: 100 mL.
Further, in S1, a purity of ethanol is 99.7%.
Further, in S2, a ratio of Mo-MI nanospheres to deionized water is 50 mg: 50 mL.
Further, in S2, an amount of the pyrrole used is 100 pL.
Further, in S2, the Mo-MI nanospheres are dispersed in deionized water and stirred for 1 h, followed by dropwise addition of 100 pL pyrrole solution and stirring for 2 h in an ice-water bath.
Beneficial effects of the present invention.
The amorphous MoO2x@C composite meterail exhibits significantly enhanced electronic conductivity, primarily attributed to the disordered nature of its amorphous structure. This disordered structure disrupts the rigid band structure characteristic of crystalline materials, leading to the formation of localized electronic states and a reduction in band gap, thereby facilitating easier Li* intercalation/deintercalation within the material.
In addition, the carbon coating further improves the conductivity of the material. The carbon materials form a conductive network in the composite material, providing a high- speed channel for electron transport, thereby greatly improving the conductiv performance of the entire composite material. This structural advantage in electron transport enables the electrode material to maintain excellent performance even under rapid charge/discharge conditions.
The amorphous structure optimizes the migration pathways of Li*, enabling Li* to transport rapidly with lower energy barriers. This is partly attributed to the lack of defects such as grain boundaries and dislocations in amorphous materials, which normally accelerrate the migration of Li+ in crystalline materials. In addition, the presence of the carbon layer not only provides physical protection, but also further reduces the resistance to Li* migration by generating an interfacial electric field effect, accelerating the intercalation and deintercalation process of lithium ions. This optimized Li* migration mechanism allows the material to maintain exceptional discharge capacity even at high current rates.
Since the intercalation/deintercalation of Li+ during the charge and discharge processes will cause the volume change of MoO» material, which typically cause structural collapse and pulverization in conventional crystalline structures.
However, the amorphous MoO2x@C provides sufficient volume expansion space buffer through the flexible coating of the carbon layer, absorbs the intrinsic stress and 06 prevents the agglomeration and rupture of the active material particles. This core-shell structure design significantly improves the structural integrity and stability of the material during multiple charge and discharge cycles. The results show that the material can still maintain a high capacity after multiple cycles, which means that its cycle life has been effectively extended.
The use of phosphomolybdic acid and pyrrole as reaction precursors and the process route of low temperature pyrolysis not only avoids the environmental burden that may be associated with high temperatures and vigorous reaction conditions, but also ensures the chemical stability of the materials. The presence of a carbon layer provides a protective barrier for the active materials and avoids excessive oxidation or dissolution due to side reactions during the electrochemical reaction, further ensuring the chemical stability and safety of the materials. In addition, the selection of chemical reagents and the process flow during the whole synthesis process are in line with the principles of green chemistry, which reduces the risk of environmental pollution and enhances the sustainability of the process.
The amorphous MoO2.x@C composite material provided by the present invention shows significant improvement in electrochemical performance, laying a solid foundation for large-scale application in energy storage devices such as lithium-ion batteries.
Of course, any product implementing of the present invention does not necessarily need to achieve all of the advantages described above at the same time.
BRIEF DESCRIPTION OF THE FIGURES
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following will briefly introduce the accompanying drawings to be used in the description of the embodiments, and it will be obvious that the accompanying drawings in the following description are only some of the embodiments of the present invention, and that for the person of ordinary skill in the field, other accompanying drawings can be obtained according to these drawings without creative labour.
Fig. 1 is an overall flow diagram of the present invention.
Fig. 2 shows the field emission scanning electron microscopy images and high- resolution transmission electron microscopy images of the carbon-coated amorphous. 601996
MoO2(MoO2x@C) prepared in Embodiment 1; (a) scanning electron microscopy image of Mo-MI precursor and (b) scanning electron microscopy image of MoO2,@C-450, (c) low-magnification transmission electron microscopy image of MoO2x@C-450, (d-e) high- resolution transmission electron microscopy images of MoO2x@C-450 and (f) high- resolution transmission electron microscopy image of MoO@C, (g-l) STEM elemental mapping images of MoO2,@C-450.
Fig. 3 shows the electrochemical performance diagrams of the carbon-coated amorphous MoO-(MoO2,@C) prepared in Embodiment 1; (a) Cyclic voltammetry (CV) curves of MoO2x@C-450, (b) Rate capability of MoO2,@C-350/450/550 and MoO.,@C, (c) Charge/discharge profiles of MoO2,@C-450 at different current densities, (d) Long- term cycling performance of MoO2x@C-450 and MoO,@C, (e) Charge/discharge curves of MoO2x@C-450 at a constant current density, (f) CV curves of MoO2.x@C-450 at various scan rates (0.1-1.0 mV s™), (g) Calculated b-values derived from the CV curves, (h) Percentage contributions of capacitive effects and diffusion-controlled effects for
MoO2x@C-450 at 0.1, 0.2, 0.5, 0.8, and 1.0 mV s™.
Fig. 4 shows electrochemical kinetic analysis and full-cell performance of the carbon- coated amorphous MoO2(MoO2x@C) prepared in Embodiment 1; (a) electrochemical impedance spectroscopy plots of MoO2,@C-350/450/550 and MoO,@C; (b) warburg factor plots in the low-frequency region; (c) galvanostatic intermittent titration technique curves of MoO>,@C-450 and MoO,@C; (d) log(Dui*) values of MoO2x@C-450 and
MoO,@C at discharged and charged states; (e) EIS spectra of MoO2x@C-450 at different cycling intervals; (f) schematic illustration of the full-cell configuration (MoO x@C-450||LCO); (g) rate capability of MoO2x@C-450||[LCO; (h) cycling performance of
MoO2.x@C-450||LCO; (i) capacity-voltage profiles of the full-cell at different cycles.
DESCRIPTION OF THE INVENTION
The technical solutions in the embodiments of the present invention will be described clearly and completely in the following in conjunction with the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention and not all of the embodiments.
Based on the embodiments in the present invention, all other embodiments obtained by a person of ordinary skill in the art without making creative labour fall within the scope 91998 of protection of the present invention.
Embodiment 1
The method of preparing an amorphous MoO2,@C composite material according to this embodiment, using phosphomolybdic acid as a molybdenum source and pyrrole (Py) as a carbon source, including the following steps.
S1: 0.06 mmol of phosphomolybdic acid is dissolved in 100 mL of ethanol. Then, 12.0 mml of 2-methylimidazole is dissolved in another 100 mL of ethanol to prepare a solution, which is then added to the phosphomolybdic acid solution. The mixed solution is allowed to stand for 24 hours. After that, the resulting precursor is collected by centrifugation and vacuum dried at 60°C for 24 hours.
S2: 50 mg of Mo-MI nanospheres are dispersed in 50 mL of deionized water and stirred for 1 hour, and then 100 uL of pyrrole solution is added dropwise and stirred in an ice-water bath for 2 hours. The solution is centrifuged to obtain the Mo-MI@PPy precursor, which is vacuum dried at 60°C for 24 hours.
S3: The prepared Mo-MI@PPy precursor is pyrolyzed under a nitrogen atmosphere at 450°C for 2 hours to obtain carbon-coated amorphous MoO2(MoO2.x@C).
Embodiment 2
The method of preparing an amorphous MoO2,@C composite material according to this embodiment, using phosphomolybdic acid as a molybdenum source and dopamine hydrochloride (PDA) as a carbon source, including the following steps.
S1: 0.06 mmol of phosphomolybdic acid is dissolved in 100 mL of ethanol. Then, 12.0 mml of 2-methylimidazole is dissolved in another 100 mL of ethanol to prepare a solution, which is then added to the phosphomolybdic acid solution. The mixed solution is allowed to stand for 24 hours. After that, the resulting precursor is collected by centrifugation and vacuum dried at 60°C for 24 hours.
S2: 50 mg of Mo-MI nanospheres are dispersed in 50 mL of Tris buffer (10 x 10-3
M) and stirred for 1 hour, and then 50 mg of PDA is added to the mixture. After stirring the solution for 24 hours, the solution is centrifuged to obtain the Mo-MI@PDA precursor.
The collected material is vacuum dried at 60°C for 24 hours.
S3: The prepared Mo-MI@PDA precursor is pyrolyzed under a nitrogen atmosphere at 450°C for 2 hours to obtain carbon-coated amorphous MoO. (denoted as MoO. x@PDA).
Embodiment 3 17001998
The method of preparing an amorphous MoO2,@C composite material according to this embodiment, using phosphomolybdic acid as a molybdenum source and polyacrylonitrile (PAN) as a carbon source, including the following steps.
S1: 0.06 mmol of phosphomolybdic acid is dissolved in 100 mL of ethanol. Then, 12.0 mml of 2-methylimidazole is dissolved in another 100 mL of ethanol to prepare a solution, which is then added to the phosphomolybdic acid solution. The mixed solution is allowed to stand for 24 hours. After that, the resulting precursor is collected by centrifugation and vacuum dried at 60°C for 24 hours.
S2: 0.5 g of PAN is added to 5.0 mL of N,N-dimethylformamide. Subsequently, 0.15 g of the prepared Mo-MI precursor is dispersed into the solution and stirred vigorously for 24 h to ensure uniformity. Finally, the homogeneous solution is loaded into a 5 mL syringe and electrospun at 20 kV to form Mo-MI@CNF precursor.
S3: The prepared Mo-MI@PDA precursor is pyrolyzed under a nitrogen atmosphere at 450°C for 2 hours to obtain carbon-coated amorphous MoO. (denoted as MoO. x@CNF).
The above disclosed preferred embodiments of the invention are intended only to aid in the description of the invention. The preferred embodiments are not intended to be exhaustive in detail, nor do they limit the invention to the specific embodiments described.
Obviously, many modifications and variations may be made in accordance with the contents of this specification. These embodiments are selected and described in this specification to better explain the principles and practical applications of the present invention, and to enable those skilled in the art to understand and utilise the present invention. The present invention is limited only by the claims and their entire scope and equivalents.

Claims (7)

CLAIMS LU601996
1. A method of preparing an amorphous MoO2,@C composite material, characterized in that phosphomolybdic acid is used as a molybdenum source and pyrrole as a carbon source, comnprising following steps: S1: dissolving phosphomolybdic acid in ethanol to prepare a phosphomolybdic acid ethanol solution; subsequently, dissolving 2-methylimidazole in another portion of ethanol to form a 2-methylimidazole ethanol solution and then adding to the phosphomolybdic acid ethanol solution; then, allowing the mixed solution to stand, and collecting the resulting Mo-MI precursor by centrifugation; S2: dispersing the Mo-MI precursor nanospheres obtained in S1 in deionized water, followed by stirring; then, dropwise adding a pyrrole solution and continuously stirring in an ice-water bath; subsequently, performing centrifugation to obtain a polypyrrole-coated Mo-MI (Mo-MI@PPYy) precursor, followed by vacuum-drying the precursor at 60°C for 24 hours; and S3: subjecting the dried Mo-MI@PPy precursor to pyrolysis at 450°C for 2 hours under a nitrogen atmosphere, thereby obtaining an amorphous MoO>,@C composite material.
2. The method of preparing the amorphous MoO2x@C composite material according to claim 1, characterized in that in S1, a ratio of phosphomolybdic acid to ethanol is 0.06 mmol: 100 mL.
3. The method of preparing the amorphous MoO2x@C composite material according to claim 1, characterized in that in S1, a ratio of 2-methylimidazole to ethanol is 12.0 mm!: 100mL.
4. The method of preparing the amorphous MoO2x@C composite material according to claim 1, characterized in that in S1, a purity of ethanol is 99.7%.
5. The method of preparing the amorphous MoO2x@C composite material according to claim 1, characterized in that in S2, a ratio of Mo-MI nanospheres to deionized water is 50 mg: 50 mL.
6. The method of preparing the amorphous MoO2x@C composite material according to claim 1, characterized in that in S2, an amount of the pyrrole used is 100 pL. 17001998
7. The method of preparing the amorphous MoO2x@C composite material according to claim 1, characterized in that in S2, the Mo-MI nanospheres are dispersed in deionized water and stirred for 1 h, followed by dropwise addition of 100 uL pyrrole solution and stirring for 2 h in an ice-water bath.
LU601996A 2024-11-14 2025-06-10 Method of preparing an amorphous moo2-x@c composite material LU601996B1 (en)

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