CN111403742A - Pod-shaped MoS2-SnO2Magnesium-lithium hybrid ion battery anode material and synthesis method and application thereof - Google Patents

Pod-shaped MoS2-SnO2Magnesium-lithium hybrid ion battery anode material and synthesis method and application thereof Download PDF

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CN111403742A
CN111403742A CN202010217399.4A CN202010217399A CN111403742A CN 111403742 A CN111403742 A CN 111403742A CN 202010217399 A CN202010217399 A CN 202010217399A CN 111403742 A CN111403742 A CN 111403742A
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侯小江
侯凯铭
石洪昌
冯雷
锁国权
叶晓慧
张荔
杨艳玲
朱建锋
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Shaanxi University of Science and Technology
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Abstract

Pod-shaped MoS2‑SnO2The magnesium-lithium hybrid ion battery anode material and the synthesis method and the application thereof comprise the following steps: SnCl2·2H2Dissolving O in a mixed solution composed of absolute ethyl alcohol and DMF to obtain a solution A; step two: dissolving PVP in the solution A to obtain solutionSolution B; step three: mixing nanometer flower-shaped MoS2Adding mineral oil into the solution B, stirring to obtain precursor solution C, and performing electrostatic spinning, wherein the flow rate of the injection pump is set to be 8m L h‑1Spraying the solution C, performing high-voltage electrostatic spinning, collecting the film on the filament collecting plate after the electrostatic spinning is finished, annealing in the air, and naturally cooling to room temperature to obtain powdery legume MoS2‑SnO2A magnesium-lithium hybrid ion battery positive electrode material sample. The invention improves the charge and discharge capacity and the dynamic characteristics of the magnesium-lithium double-salt battery, improves the cycle stability of the magnesium-lithium double-salt battery and prolongs the service life of the battery.

Description

Pod-shaped MoS2-SnO2Magnesium-lithium hybrid ion battery anode material and synthesis method and application thereof
Technical Field
The invention relates to the technical field of secondary power battery materials, in particular to a pod-shaped MoS2-SnO2A magnesium-lithium hybrid ion battery anode material and a synthesis method and application thereof.
Background
Development and utilization of energy are accompanied with development of human beings and social progress, and energy is a necessity of daily life and "drives" human life and social progress. The population is rapidly growing and the heavy industry is rapidly expanding, resulting in the rising demand for energy and the gradual appearance of environmental problems caused by the large consumption of fossil energy. However, the traditional fossil energy is not renewable and has been over-exploited, which forces the global embarrassment of depletion and environmental pollution of fossil energy, and the development and utilization of sustainable energy of clean, efficient and renewable energy and the upgrading of the current energy system are urgent. Human beings always explore respective new energy sources without residue, and actively promote energy source replacement. Every energy upgrading and upgrading means the progress of social productivity, and the social and economic development is promoted.
Energy storage materials are indispensable in the current society, and with the rapid increase of portable devices, the requirements of energy storage materials and devices are more and more urgent. As an energy storage device, lithium ion batteries have enjoyed great success in the commercial rechargeable battery market. However, the problems of limited lithium ion storage, high cost, short circuit of the battery caused by the growth of lithium dendrite, even fire hazard, limited capacity and the like compel people to need a new ion battery to replace the lithium ion battery, thereby meeting the requirements of social development. Due to low cost, no dendrite and double electron redox characteristics, high capacity (magnesium is 3833mAh cm)-3Lithium is 2046mAh cm-3) And the rechargeable magnesium ion battery has the remarkable characteristics that the rechargeable magnesium ion battery has great advantages and is a novel ion battery expected to be used in a large scale. Therefore, magnesium ion batteries have received increasing attention.
Although studies related to magnesium ion batteries have been reported, it has better Mg2+The high voltage positive electrode material with ion intercalation kinetics is very limited, which seriously hinders the application of magnesium ion batteries. Due to Mg2+The ion charge density is high, and strong coulomb acting force exists between the ion charge density and the positive material of the battery, so that Mg is seriously restricted2+The migration of ions in the cathode material results in lower electrochemical utilization rate and rate capability of the cathode material. Therefore, most of the lithium ion battery cathode materials developed at present are not suitable for magnesium ion batteries. In recent years, the problems encountered by magnesium ion batteries can be remarkably solved by constructing a lithium-magnesium double-salt battery system. The specific method is to adopt a lithium-embedded anode material, a magnesium anode material and Mg-contained2+And L i+High efficiency L i for positive electrode of battery+Ion de-intercalation reaction, and Mg generation at the negative electrode2+The dissolution and deposition reaction of the ions effectively relieves the problems of low capacity, high cost, lithium dendrite, release kinetics of the magnesium ion battery and the like of the lithium ion battery, and promotes the application of the magnesium-based energy storage battery.
At present, lithium-intercalation positive electrode materials used by lithium ion batteries and double-salt batteries have the problems of single component, simple structure, insufficient conductivity, low activity, unstable structure, lack of channels for fast ion deintercalation and the like, the fast saturated intercalation/deintercalation of lithium ions is severely restricted, and the capacity, rate characteristics and cycle stability of a battery system are reduced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a pod-shaped MoS2-SnO2The magnesium-lithium hybrid ion battery anode material, the synthesis method and the application thereof improve the charge-discharge capacity and the dynamic characteristics of the magnesium-lithium double-salt battery, improve the cycle stability of the magnesium-lithium double-salt battery and prolong the service life of the battery.
In order to achieve the purpose, the invention adopts the technical scheme that:
pod-shaped MoS2-SnO2The magnesium-lithium hybrid ion battery anode material is one-dimensional nano-tube-shaped SnO2Discontinuous intercalation of active MoS2Pod-shaped composite anode material formed by nanoflowers and one-dimensional nano-tubular SnO2The x accounts for 40-60 wt.%, and the rest is nano flower-shaped MoS2。
Pod-shaped MoS2-SnO2The synthesis method of the magnesium-lithium hybrid ion battery anode material comprises the following steps;
the method comprises the following steps:
1.5-2.0 g SnCl2·2H2Dissolving O in a mixed solution consisting of 1.0-3.0 g of absolute ethyl alcohol and 1.0-3.0 g of DMF, and stirring to obtain a solution A;
step two:
dissolving 0.2-0.6 g of PVP in the solution A, and continuously stirring to obtain a solution B;
step three:
0.1-0.4 g of nano flower-shaped MoS2Adding 0.2g of mineral oil into the solution B, stirring to obtain a precursor solution C, and carrying out electrostatic spinning;
step four:
a plain end needle with an internal diameter of 0.5mm was attached to the syringe as a spinneret, a stainless steel mesh plate grounded to the power supply as a take-up screen, held between the spinneret and a collection plateThe distance between the two was 20cm and a high voltage of 18kV was applied, and the flow rate of the injection pump was set at 8m L. h-1Spraying the solution C, performing high-voltage electrostatic spinning, after the electrostatic spinning is finished, collecting the film on the yarn collecting plate, and performing annealing treatment in the air, wherein the annealing temperature is 480 ℃, the time is 3 hours, and the heating rate is 5 ℃ per minute-1Naturally cooling to room temperature to obtain powdery legume MoS2-SnO2A magnesium-lithium hybrid ion battery positive electrode material sample.
In the first step, stirring is carried out at room temperature for 1.5-2.5 h at 800 rap/min.
And in the second step, stirring is continuously carried out for 4-6 h at room temperature of 800 rap/min.
And in the third step, stirring at room temperature for 24-48 h at 800 rap/min.
Legume MoS2-SnO2The application of the positive electrode material of the magnesium-lithium hybrid ion battery is to mix 70 wt.% of pod-shaped MoS2-SnO2The method comprises the steps of putting a magnesium-lithium hybrid ion battery positive electrode material sample, 15 wt.% of conductive additive (Super P) and 15 wt.% of polyvinylidene fluoride (PVDF) binder into a mortar for full grinding, coating mixed sample slurry on copper foil by a scraper, then putting the copper foil into a vacuum oven at 110 ℃ for drying for 12 hours to enable the copper foil to be fully dried, taking a glass fiber diaphragm as a battery diaphragm to assemble a button cell, standing the assembled button cell for 12 hours, and then carrying out electrochemical performance test on L ANDCT2100A, wherein the test voltage is 0.01-3.0V, and the current density is 100 mA/g.
The invention has the beneficial effects that:
the invention provides a pod-shaped MoS2-SnO2The positive electrode material of the magnesium-lithium hybrid ion battery is prepared by one-step high-voltage electrostatic method on one-dimensional SnO with good conductivity2Discontinuous embedding of high activity MoS in nanotubes2Flower-like material to synthesize a pod-like MoS2-SnO2A magnesium-lithium hybrid ion battery anode material. By means of tubular highly conductive SnO2The one-dimensional material can rapidly realize the migration of electrons and lithium ions by means of high-activity MoS2MoS in nanoflower active materials2Interlayer spacing for storing lithium ions and improving magnesium-lithium double salt electricityThe charge and discharge capacity and the dynamic characteristics of the cell. In addition, the carbon fiber carries MoS2The problem of material pulverization caused by volume expansion/contraction of the anode material due to L i + intercalation/deintercalation can be effectively relieved, so that the cycling stability of the magnesium-lithium double-salt battery is improved, and the service life of the battery is prolonged.
Using magnesium as battery cathode, and bean-shaped MoS2-SnO2The magnesium-lithium hybrid ion battery is used as a positive electrode material and is matched with L i+And Mg2+And double-salt electrolyte with coexisting ions forms the magnesium-lithium hybrid ion battery. During the charge and discharge process, Mg is generated on the negative electrode side of the metal magnesium2+Deposition and elution reactions of ions, and L i is mainly generated on the positive electrode material side+The ion extraction/insertion reaction in the material. Pod-shaped MoS prepared by the invention2-SnO2The positive electrode material of Mg-Li hybridized ion battery can fully utilize SnO2High conductivity of L i+And fast migration and MoS of electrons2High activity and layered microstructure efficient storage L i+The pod-shaped structure formed by discontinuous dispersion is beneficial to smooth transmission and storage of L i +, and relieving expansion/contraction stress, and improves the charge-discharge electrodynamics characteristic, the capacity characteristic and the cycle stability of the battery.
Drawings
FIG. 1 is a diagram of a legume MoS of the present invention2-SnO2A microscopic morphology picture of the cathode material of the magnesium-lithium hybrid ion battery.
Detailed Description
The present invention will be described in further detail with reference to examples.
FIG. 1 is a diagram of a legume-like MoS synthesized in the present invention2-SnO2The microstructure morphology of the cathode material of the magnesium-lithium hybrid ion battery can be seen from the figure, the hydrothermal and electrostatic spinning synthesis process has good effect, and the legume-like MoS is synthesized2-SnO2A battery positive electrode material. One-step hydrothermal synthesis process has good effect, and nano MoS formed by hydrothermal synthesis2SnO capable of being uniformly distributed in high-voltage electrostatic spinning preparation2In the nanotube, a typical pod-like structure morphology is formed.
SnO with good conductivity by high-voltage electrostatic spinning method2Hydrothermal synthesis active MoS embedded in one-dimensional nanotube2Nanoflower, by subsequent annealing, to form a pod-like MoS2-SnO2A magnesium-lithium hybrid ion battery anode material. By means of tubular highly conductive SnO2The one-dimensional material can rapidly realize the migration of electrons and lithium ions by means of high-activity MoS2MoS in nanoflower active materials2The interlayer space stores lithium ions, and the charge and discharge capacity and the dynamic characteristics of the magnesium-lithium double-salt battery are improved. In addition, the carbon fiber carries MoS2The problem of material pulverization caused by volume expansion/contraction of the anode material due to L i + intercalation/deintercalation can be effectively relieved, so that the cycling stability of the magnesium-lithium double-salt battery is improved, and the service life of the battery is prolonged.
In order to improve the conductivity of the positive electrode material of the magnesium-lithium double-salt battery and improve the lithium ion releasing/inserting characteristics of the positive electrode material, the characteristics of high charge-discharge efficiency of a magnesium negative electrode, no generation of dendrites, stable structure and excellent dynamic properties of the lithium inserting positive electrode material are fully exerted, good electrochemical charge-discharge characteristics are shown, and the power battery with high capacity, safety and long service life is prepared.
Example 1:
pod-shaped MoS2-SnO2A magnesium-lithium hybrid ion battery anode material and a synthesis method thereof.
Pod-shaped MoS2-xSnO2The magnesium-lithium hybrid ion battery anode material is one-dimensional nano-tube-shaped SnO2Discontinuous intercalation of active MoS2Pod-shaped composite anode material formed by nanoflowers and one-dimensional nano-tubular SnO2The x accounts for 40-60 wt.%, and the rest is nano flower-shaped MoS2。
Pod-shaped MoS2-xSnO2The synthesis method of the magnesium-lithium hybrid ion battery cathode material comprises the following steps of (1) mixing x is 40 wt%;
the method comprises the following steps:
1.5g SnCl2·2H2Dissolving O in a mixed solution consisting of 1.0g of absolute ethyl alcohol and 1.0g of DMF, and stirring at room temperature for 1.5h at 800rap/min to obtain a solution A;
step two:
dissolving 0.2g of PVP in the solution A, and continuously stirring at room temperature for 4 hours at 800rap/min to obtain a solution B;
step three:
0.4g of nano flower-like MoS2Adding 0.2g of mineral oil into the solution B, stirring at room temperature of 800rap/min for 24 hours to obtain a precursor solution C, and carrying out electrostatic spinning;
step four:
a plain end needle with an inner diameter of 0.5mm was connected to the syringe as a spinneret, a stainless steel mesh plate with a grounded power supply as a wire collecting net, the distance between the spinneret and the collecting plate was kept at 20cm and a high voltage of 18kV was applied between them, and the flow rate of the injection pump was set at 8m L. h-1Spraying the solution C, performing high-voltage electrostatic spinning, after the electrostatic spinning is finished, collecting the film on the yarn collecting plate, and performing annealing treatment in the air, wherein the annealing temperature is 480 ℃, the time is 3 hours, and the heating rate is 5 ℃ per minute-1Naturally cooling to room temperature to obtain powdery legume MoS2-SnO2A magnesium-lithium hybrid ion battery positive electrode material sample.
Legume MoS2-SnO2The application of the positive electrode material of the magnesium-lithium hybrid ion battery is to mix 70 wt.% of pod-shaped MoS2-SnO2The method comprises the steps of putting a magnesium-lithium hybrid ion battery positive electrode material sample, 15 wt.% of conductive additive (Super P) and 15 wt.% of polyvinylidene fluoride (PVDF) binder into a mortar for full grinding, coating mixed sample slurry on copper foil by a scraper, then putting the copper foil into a vacuum oven at 110 ℃ for drying for 12 hours to enable the copper foil to be fully dried, taking a glass fiber diaphragm as a battery diaphragm to assemble a button cell, standing the assembled button cell for 12 hours, and then carrying out electrochemical performance test on L ANDCT2100A, wherein the test voltage is 0.01-3.0V, and the current density is 100 mA/g.
Example 2:
pod-shaped MoS2-SnO2A magnesium-lithium hybrid ion battery anode material and a synthesis method thereof.
Pod-shaped MoS2-xSnO2The magnesium-lithium hybrid ion battery anode material is one-dimensional nano-tube-shaped SnO2Discontinuous intercalation of active MoS2Pod-shaped composite anode material formed by nanoflowers and one-dimensional nano-tubular SnO2The x accounts for 40-60 wt.%, and the rest is nano flower-shaped MoS2。
Pod-shaped MoS2-xSnO2The synthesis method of the magnesium-lithium hybrid ion battery cathode material comprises the following steps of (1) mixing x is 50 wt.%;
the method comprises the following steps:
1.75g of SnCl2·2H2Dissolving O in a mixed solution consisting of 2.0g of absolute ethyl alcohol and 2.0g of DMF, and stirring at room temperature for 2 hours at 800rap/min to obtain a solution A;
step two:
dissolving 0.4g of PVP in the solution A, and continuously stirring at the room temperature for 5 hours at 800rap/min to obtain a solution B;
step three:
0.25g of nano flower-like MoS2Adding 0.2g of mineral oil into the solution B, stirring at room temperature of 800rap/min for 36 hours to obtain a precursor solution C, and carrying out electrostatic spinning;
step four:
a plain end needle with an inner diameter of 0.5mm was connected to the syringe as a spinneret, a stainless steel mesh plate with a grounded power supply as a wire collecting net, the distance between the spinneret and the collecting plate was kept at 20cm and a high voltage of 18kV was applied between them, and the flow rate of the injection pump was set at 8m L. h-1Spraying the solution C, performing high-voltage electrostatic spinning, after the electrostatic spinning is finished, collecting the film on the yarn collecting plate, and performing annealing treatment in the air, wherein the annealing temperature is 480 ℃, the time is 3 hours, and the heating rate is 5 ℃ per minute-1Naturally cooling to room temperature to obtain powdery legume MoS2-SnO2A magnesium-lithium hybrid ion battery positive electrode material sample.
Legume MoS2-SnO2The application of the positive electrode material of the magnesium-lithium hybrid ion battery is to mix 70 wt.% of pod-shaped MoS2-SnO2Putting a magnesium-lithium hybrid ion battery positive electrode material sample, 15 wt.% of conductive additive (Super P) and 15 wt.% of polyvinylidene fluoride (PVDF) binder into a mortar for full grinding, and coating the mixed sample slurry by using a scraperAnd standing the assembled button cell for 12 hours, and then carrying out an electrochemical performance test on L ANDCT2100A, wherein the test voltage is 0.01-3.0V, and the current density is 100 mA/g.
Example 3:
pod-shaped MoS2-SnO2A magnesium-lithium hybrid ion battery anode material and a synthesis method thereof.
Pod-shaped MoS2-xSnO2The magnesium-lithium hybrid ion battery anode material is one-dimensional nano-tube-shaped SnO2Discontinuous intercalation of active MoS2Pod-shaped composite anode material formed by nanoflowers and one-dimensional nano-tubular SnO2The x accounts for 40-60 wt.%, and the rest is nano flower-shaped MoS2。
Pod-shaped MoS2-xSnO2The synthesis method of the magnesium-lithium hybrid ion battery cathode material comprises the following steps of (1) mixing x 60 wt%;
the method comprises the following steps:
2.0g of SnCl2·2H2Dissolving O in a mixed solution consisting of 3.0g of absolute ethyl alcohol and 3.0g of DMF, and stirring at room temperature for 2.5 hours at 800rap/min to obtain a solution A;
step two:
dissolving 0.6g of PVP in the solution A, and continuously stirring at room temperature for 6h at 800rap/min to obtain a solution B;
step three:
0.1g of nano flower-like MoS2Adding 0.2g of mineral oil into the solution B, stirring at room temperature of 800rap/min for 48h to obtain a precursor solution C, and carrying out electrostatic spinning;
step four:
a plain end needle with an inner diameter of 0.5mm was connected to the syringe as a spinneret, a stainless steel mesh plate with a grounded power supply as a wire collecting net, the distance between the spinneret and the collecting plate was kept at 20cm and a high voltage of 18kV was applied between them, and the flow rate of the injection pump was set at 8m L. h-1Spraying the solution C, performing high-voltage electrostatic spinning, and collecting the film on the filament collecting plate after the electrostatic spinning is finishedAnnealing in air at 480 deg.C for 3 hr at a temperature of 5 deg.C/min-1Naturally cooling to room temperature to obtain powdery legume MoS2-SnO2A magnesium-lithium hybrid ion battery positive electrode material sample.
Legume MoS2-SnO2The application of the positive electrode material of the magnesium-lithium hybrid ion battery is to mix 70 wt.% of pod-shaped MoS2-SnO2The method comprises the steps of putting a magnesium-lithium hybrid ion battery positive electrode material sample, 15 wt.% of conductive additive (Super P) and 15 wt.% of polyvinylidene fluoride (PVDF) binder into a mortar for full grinding, coating mixed sample slurry on copper foil by a scraper, then putting the copper foil into a vacuum oven at 110 ℃ for drying for 12 hours to enable the copper foil to be fully dried, taking a glass fiber diaphragm as a battery diaphragm to assemble a button cell, standing the assembled button cell for 12 hours, and then carrying out electrochemical performance test on L ANDCT2100A, wherein the test voltage is 0.01-3.0V, and the current density is 100 mA/g.

Claims (6)

1. Pod-shaped MoS2-SnO2The magnesium-lithium hybrid ion battery anode material is characterized by being one-dimensional nano-tube-shaped SnO2Discontinuous intercalation of active MoS2Pod-shaped composite anode material formed by nanoflowers and one-dimensional nano-tubular SnO2The x accounts for 40-60 wt.%, and the rest is nano flower-shaped MoS2。
2. Pod-shaped MoS2-SnO2The synthesis method of the magnesium-lithium hybrid ion battery anode material is characterized by comprising the following steps;
the method comprises the following steps:
1.5-2.0 g SnCl2·2H2Dissolving O in a mixed solution consisting of 1.0-3.0 g of absolute ethyl alcohol and 1.0-3.0 g of DMF, and stirring to obtain a solution A;
step two:
dissolving 0.2-0.6 g of PVP in the solution A, and continuously stirring to obtain a solution B;
step three:
0.1-0.4 g of nano flower-shaped MoS2Adding 0.2g of mineral oil into the solution B, stirring to obtain a precursor solution C, and carrying out electrostatic spinning;
step four:
a plain end needle with an inner diameter of 0.5mm was connected to the syringe as a spinneret, a stainless steel mesh plate with a grounded power supply as a wire collecting net, the distance between the spinneret and the collecting plate was kept at 20cm and a high voltage of 18kV was applied between them, and the flow rate of the injection pump was set at 8m L. h-1Spraying the solution C, performing high-voltage electrostatic spinning, after the electrostatic spinning is finished, collecting the film on the yarn collecting plate, and performing annealing treatment in the air, wherein the annealing temperature is 480 ℃, the time is 3 hours, and the heating rate is 5 ℃ per minute-1Naturally cooling to room temperature to obtain powdery legume MoS2-SnO2A magnesium-lithium hybrid ion battery positive electrode material sample.
3. A pod-like MoS according to claim 22-SnO2The method for synthesizing the magnesium-lithium hybrid ion battery anode material is characterized in that in the step I, the material is stirred for 1.5-2.5 hours at room temperature of 800 rap/min.
4. A pod-like MoS according to claim 22-SnO2The synthesis method of the magnesium-lithium hybrid ion battery anode material is characterized in that in the second step, the stirring is continued for 4-6 hours at room temperature of 800 rap/min.
5. A pod-like MoS according to claim 22-SnO2The synthesis method of the magnesium-lithium hybrid ion battery anode material is characterized in that in the third step, 800rap/min is stirred at room temperature for 24-48 h.
6. Legume MoS2-SnO2The application of the positive electrode material of the magnesium-lithium hybrid ion battery is to mix 70 wt.% of pod-shaped MoS2-SnO2Putting a magnesium-lithium hybrid ion battery positive electrode material sample, 15 wt.% of conductive additive (Super P) and 15 wt.% of polyvinylidene fluoride (PVDF) binder into a mortar for full grinding, and scraping the mixed sample slurryAnd standing the assembled button cell for 12 hours, and then carrying out an electrochemical performance test on L ANDCT2100A, wherein the test voltage is 0.01-3.0V, and the current density is 100 mA/g.
CN202010217399.4A 2020-03-25 2020-03-25 Pod-shaped MoS2-SnO2Magnesium-lithium hybrid ion battery anode material and synthesis method and application thereof Pending CN111403742A (en)

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