CN110571436A - Preparation method of three-dimensional porous carbon loaded flaky molybdenum disulfide current collector for lithium metal cathode - Google Patents
Preparation method of three-dimensional porous carbon loaded flaky molybdenum disulfide current collector for lithium metal cathode Download PDFInfo
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Abstract
The invention relates to a preparation method of a three-dimensional porous carbon loaded flaky molybdenum disulfide current collector for a lithium metal cathode, which comprises the following steps: (1) adding a molybdenum source, a sulfur source, a carbon source and a salt template into deionized water for dissolving to prepare a uniform and transparent precursor solution; (2) freeze drying to obtain dry solid powder, and grinding to obtain a mixed powder precursor; (3) is arranged in a hearth of the tubular furnace; heating to 500-750 ℃ in an inert gas atmosphere, preserving heat for a period of time, and then rapidly cooling to obtain a calcined product; (4) carrying out suction filtration, removing NaCl, and drying to obtain the three-dimensional porous carbon loaded flaky molybdenum disulfide material; (5) and preparing the three-dimensional porous carbon loaded flaky molybdenum disulfide composite current collector.
Description
Technical Field
The invention belongs to the technical field of electrode materials of lithium metal batteries, and particularly relates to a preparation method of a three-dimensional porous carbon loaded molybdenum disulfide current collector, which can effectively inhibit the generation of lithium dendrites, the disordered deposition problem of lithium metal and the problem of battery capacity attenuation caused by further generation of dead lithium in the deposition and desorption process of the lithium metal.
Background
with the rapid development of electric vehicles, household electronic products and national power grids, people have higher and higher requirements on rechargeable batteries with high energy density, and the traditional lithium ion batteries cannot meet the energy storage requirements of people due to the problems of working principles, raw materials, modern scientific technology and the like. In this context, lithium metal has the highest theoretical specific capacity (3860mAh g)-1) Lowest electrochemical potential (3.04V vs. standard hydrogen electrode) and very low density (0.53g cm)-3) And the like, and become the most promising next-generation high energy density battery anode material, especially for lithium-sulfur and lithium-oxygen battery systems. However, problems such as repeated consumption of lithium metal and electrolyte due to formation of an unstable solid electrolyte membrane, reduction in coulombic efficiency and service life of a battery, penetration of a battery separator by growth of uncontrollable lithium dendrites to cause short-circuiting of the battery, destruction of a battery structure due to large volume expansion, etc. cause serious safety and recycling problems, hindering practical application of a lithium metal negative electrode.
The ordered deposition of lithium metal is guided, the growth of lithium dendrite and the volume expansion in the lithium deposition and desorption process are inhibited, and the coulombic efficiency and the cycle life of the lithium metal negative electrode can be effectively improved. In recent years, the support of lithium-philic seeds on a three-dimensional porous current collector has been widely used for lithium metal negative electrodes. On one hand, the three-dimensional current collector has high specific surface area, so that the local current density of the electrode can be effectively reduced, and the lithium metal deposition is more uniform; on the other hand, the porous structure has enough space to store lithium, inhibiting the growth of lithium dendrites. While the lithium-philic seeds may guide the uniform deposition of lithium metal throughout the interior of the current collector. However, the current research mainly includes that a granular lithium-philic material or a secondary supported flaky lithium-philic material is not strongly bonded with a matrix, and the lithium-philic material may fall off from the matrix or even agglomerate in the process of deposition and desorption of lithium metal, so that the uneven distribution of the lithium-philic material can promote the uneven deposition of the lithium metal, reduce the coulombic efficiency of the battery and prolong the service life of the battery.
Therefore, the problem can be effectively solved by preparing the flaky molybdenum disulfide lithium-philic material loaded on the three-dimensional porous carbon current collector with large specific surface area through a one-step method. The sheet structure is used to increase the contact area between the lithium-philic material and the substrate to improve the bonding force, so that the structure of the electrode is maintained in a long cycle. The lithium-philic material promotes the uniform deposition of lithium metal, the three-dimensional porous current collector provides a large specific surface area to reduce the relative current density and holes for storing lithium, and finally the lithium metal battery cathode material with excellent electrochemical performance is obtained.
Disclosure of Invention
aiming at the defects in the prior art, the invention aims to provide a three-dimensional porous carbon loaded molybdenum disulfide current collector which can effectively guide lithium metal to be uniformly deposited in the current collector and inhibit the generation of lithium dendrites for a lithium metal battery, and can effectively improve the coulombic efficiency and the cycling stability of the battery. The technical scheme is as follows:
A preparation method of a three-dimensional porous carbon loaded flaky molybdenum disulfide current collector for a lithium metal negative electrode comprises the following steps:
(1) Taking one or more of sucrose, glucose, citric acid and starch as a carbon source, ammonium molybdate as a molybdenum source, thiourea as a sulfur source, one or more of sodium sulfate, sodium chloride, sodium carbonate and sodium silicate as a template, and taking the molar ratio of molybdenum atoms in the molybdenum source, sulfur atoms in the sulfur source and carbon atoms in the carbon source as 1: (2-10): (50-500), adding a molybdenum source, a sulfur source, a carbon source and a salt template into deionized water for dissolving to prepare a uniform and transparent precursor solution;
(2) Freeze-drying the precursor solution prepared in the last step to obtain dry solid powder, and grinding to obtain a mixed powder precursor;
(3) Placing the mixed powder precursor obtained in the last step into a tubular furnace hearth; heating to 500-750 ℃ at a heating rate of 1-10 ℃ in an inert gas atmosphere, preserving heat for a period of time, and then rapidly cooling to obtain a calcined product;
(4) Carrying out suction filtration on the calcined product obtained in the last step by using deionized water, removing NaCl, and drying to obtain a three-dimensional porous carbon loaded flaky molybdenum disulfide material;
(5) Mixing the three-dimensional porous carbon loaded flaky molybdenum disulfide material prepared in the step (4) with polyvinylidene fluoride (PVDF) by the ratio of 8: and (1) mixing the materials according to the mass ratio, adding a proper amount of N-methyl pyrrolidone (NMP) to prepare slurry, uniformly mixing the slurry, coating the slurry on a copper foil, and drying to obtain the three-dimensional porous carbon loaded flaky molybdenum disulfide composite current collector.
in the step (3), the average cooling speed is 50-100 ℃/min.
compared with the prior art, the method has the following advantages: (1) the three-dimensional porous carbon loaded flaky molybdenum disulfide composite material is prepared by a one-step method, and the contact area between three-dimensional carbon and flaky molybdenum disulfide is very large, so that the three-dimensional carbon and the flaky molybdenum disulfide are combined very tightly, and the molybdenum disulfide is not easy to change in position and shape in the circulation process of a lithium metal battery; (2) the molybdenum disulfide can effectively improve the lithium affinity of the three-dimensional carbon matrix and promote the uniform deposition of lithium metal in the whole three-dimensional current collector; (3) the three-dimensional porous structure can contain a large amount of lithium metal, so that the volume change of the lithium metal negative electrode in the charging and discharging process can be slowed down, and the lithium metal negative electrode with stable volume is obtained; (4) the three-dimensional pore structure increases the specific surface area of the electrode and reduces the effective current density of the electrode, thereby effectively inhibiting the generation of lithium dendrites.
drawings
FIG. 1 shows MoS obtained in example 1 of the present invention2@3DC powder SEM images;
FIG. 2 is a MoS prepared according to example 1 of the present invention2TEM image of @3DC powder;
FIG. 3 is a MoS prepared in example 1 of the present invention2Deposition of 2.0mAh cm on @3DC Current collector-2And 5.0mAh cm-2SEM image of lithium metal;
FIG. 4 shows MoS obtained in example 12@3DC current collector is used to support the cyclic coulombic efficiency of lithium metal.
Nothing in this specification is said to apply to the prior art.
Specific examples of the production method of the present invention are given below. These examples are only intended to illustrate the preparation process of the present invention in detail and do not limit the scope of protection of the claims of the present application.
Detailed Description
the technical route of the invention is described below:
MoS2The preparation method of the @3DC composite current collector adopts the following process:
(1) Taking one or more of sucrose, glucose, citric acid and starch as a carbon source, ammonium molybdate as a molybdenum source, thiourea as a sulfur source, one or more of sodium sulfate, sodium chloride, sodium carbonate and sodium silicate as a template, and taking the molar ratio of molybdenum atoms in the molybdenum source, sulfur atoms in the sulfur source and carbon atoms in the carbon source as 1: (2-10): (50-500) adding a molybdenum source, a sulfur source, a carbon source and a salt template into deionized water for dissolving, preparing a solution, and stirring for more than 3 hours to obtain a uniform and transparent precursor solution;
(2) Freezing the precursor solution prepared in the last step in a refrigerator at-20 ℃ for more than 48h or rapidly freezing the precursor solution by using liquid nitrogen, then placing the precursor solution in a vacuum freeze dryer at-50 ℃ and 20Pa for about 48h to obtain dry solid powder, and grinding the dry solid powder to obtain a mixed powder precursor;
(3) Spreading about 10g of the powder precursor obtained in the last step on a quartz boat, and then placing the quartz boat in a tubular furnace hearth; with N2taking one or a mixed gas of He and Ar as an inert gas source, introducing the inert gas at a flow rate of 500ccm for 10-20 minutes to remove air, taking the inert gas as a carrier gas, fixing the flow rate at 50-500 ccm, heating to 500-750 ℃ at a heating rate of 1-10 ℃, preserving heat for 1-2 hours, and then rapidly cooling (the average cooling rate is 50-100 ℃/min) to obtain a calcined product;
(4) Carrying out suction filtration on the calcined product obtained in the last step by using deionized water, removing NaCl, and then drying in a vacuum drying oven at 70 ℃ to obtain a three-dimensional porous carbon loaded flaky molybdenum disulfide material;
(5) mixing the three-dimensional porous carbon loaded flaky molybdenum disulfide material prepared in the step (4) with polyvinylidene fluoride (PVDF) by the ratio of 8: and (1) mixing the components according to the mass ratio, adding a proper amount of N-methyl pyrrolidone (NMP) to prepare slurry, magnetically stirring for more than 4 hours, uniformly coating a scraper with the thickness of 100-1000 mm on a copper foil, drying the copper foil at 50-80 ℃ by using a heating table, and cutting the copper foil into wafers by using a cutting machine to obtain the three-dimensional porous carbon loaded flaky molybdenum disulfide composite current collector.
(6) Assembling the three-dimensional porous carbon loaded flaky molybdenum disulfide composite current collector prepared in the step (5) into a battery, wherein a counter electrode is a lithium sheet, and firstly, the voltage is 0.05mA cm within the voltage range of 0.01V-3V-2Circulating the current density for 5 circles to form a stable SEI film, and then circulating the current density for 1.0-10.0 mA cm-2The lithium metal is deposited for 0.2-10 h at the current density, and the battery is disassembled to obtain the lithium metal cathodes with different capacities.
example 1
(1) 0.3532g of ammonium molybdate, 0.3654g of thiourea, 1.4g of citric acid and 17.55g of sodium chloride are weighed out, the mixture is dissolved in 100ml of deionized water and stirred magnetically for 4 hours to obtain a homogeneous solution. Pouring the uniformly mixed liquid into a culture dish, and then freezing the culture dish for 24 hours in a refrigerator at the temperature of-20 ℃; freeze-drying the frozen sample in a freeze-dryer under the following conditions: -50 ℃, 20Pa, lyophilization time 24 h. Grinding the freeze-dried sample to obtain precursor composite powder (the particle size of the powder is 100 meshes); putting 10g of the powder into a square boat, putting the square boat into a tubular furnace, introducing 500ccm argon for 15min to remove air, adjusting the temperature to 200ccm, heating to 750 ℃ at a heating rate of 10 ℃/min, preserving heat for 2h, quickly cooling to room temperature after heat preservation, putting the calcined powder into a 500ml beaker, adding 400ml of deionized water, magnetically stirring for 30min to completely dissolve sodium chloride in water, then carrying out suction filtration, repeatedly carrying out three times, putting the suction-filtered sample into a 70 ℃ vacuum oven, and drying for 3h to obtain the three-dimensional porous carbon loaded molybdenum disulfide composite material.
(2) With the prepared powder material, the mass ratio of polyvinylidene fluoride is 8: adding a proper amount of NMP, mixing and stirring for 4 hours, coating the mixture on a copper foil by a 250mm scraper, and drying at 80 ℃ to obtain a current collector.
(3) Using MoS2Preparation of a lithium metal negative electrode of @3 DC. The current collector prepared above was used as the cathode and lithium metal as the anode to assemble a half cell, in MoS2Deposition of 2.0mAh cm on @3DC Current collector-2The battery is disassembled to obtain the corresponding lithium metal cathode.
(4) And assembling the lithium metal secondary battery. And assembling the prepared lithium metal cathode and a proper sulfur anode into a lithium sulfur battery or assembling the lithium metal cathode and a proper LMO (L is lithium, M is transition metal, and O is oxygen) into a Li-LMO battery. In this example, a lithium metal half cell was assembled using lithium metal as the counter electrode.
(5) Electrochemical testing of lithium metal secondary batteries. Firstly, the voltage is in the range of 0.01V to 3V and 0.05mA cm-2Current density of (2) was cycled for 5 cycles to obtain a stable SEI film, then at 1.0mA cm-2Current density of 2.0mAh cm-2The capacity of (2) was subjected to charge-discharge cycles, and the cut-off voltage was 0.5V.
Example 2
The difference from example 1 is: (1) 0.3532g of ammonium molybdate, 0.30g of thiourea, 1.4g of citric acid and 17.55g of sodium chloride were weighed, the mixture was dissolved in 100ml of deionized water, and magnetic stirring was carried out for 4 hours to obtain a uniform solution. Pouring the uniformly mixed liquid into a culture dish, and then freezing the culture dish for 24 hours in a refrigerator at the temperature of-20 ℃; freeze-drying the frozen sample in a freeze-dryer under the following conditions: -50 ℃, 20Pa, lyophilization time 24 h. Grinding the freeze-dried sample to obtain precursor composite powder (the particle size of the powder is 100 meshes); putting 10g of the powder into a square boat, putting the square boat into a tubular furnace, introducing 500ccm argon for 15min to remove air, adjusting the temperature to 200ccm, heating to 750 ℃ at a heating rate of 10 ℃/min, preserving heat for 2h, quickly cooling to room temperature after heat preservation, putting the calcined powder into a 500ml beaker, adding 400ml of deionized water, magnetically stirring for 30min to completely dissolve sodium chloride in water, then carrying out suction filtration, repeatedly carrying out three times, putting the suction-filtered sample into a 70 ℃ vacuum oven, and drying for 3h to obtain the three-dimensional porous carbon loaded molybdenum disulfide composite material. The rest is the same as embodiment 1, and the description is omitted here.
the resulting current collector had a three-dimensional porous structure, but had many particles on the carbon wall, presumably left by incomplete sulfidation of the molybdenum oxide from the decomposition of ammonium molybdate with thiourea.
example 3
the difference from example 1 is: (1) 0.3532g of ammonium molybdate, 0.3654g g g of thiourea, 1g of citric acid and 17.55g of sodium chloride are weighed out, the mixture is dissolved in 100ml of deionized water and stirred magnetically for 4 hours to obtain a homogeneous solution. Pouring the uniformly mixed liquid into a culture dish, and then freezing the culture dish for 24 hours in a refrigerator at the temperature of-20 ℃; freeze-drying the frozen sample in a freeze-dryer under the following conditions: -50 ℃, 20Pa, lyophilization time 24 h. Grinding the freeze-dried sample to obtain precursor composite powder (the particle size of the powder is 100 meshes); putting 10g of the powder into a square boat, putting the square boat into a tubular furnace, introducing 500ccm argon for 15min to remove air, adjusting the temperature to 200ccm, heating to 750 ℃ at a heating rate of 10 ℃/min, preserving heat for 2h, quickly cooling to room temperature after heat preservation, putting the calcined powder into a 500ml beaker, adding 400ml of deionized water, magnetically stirring for 30min to completely dissolve sodium chloride in water, then carrying out suction filtration, repeatedly carrying out three times, putting the suction-filtered sample into a 70 ℃ vacuum oven, and drying for 3h to obtain the three-dimensional porous carbon loaded molybdenum disulfide composite material. The rest is the same as embodiment 1, and the description is omitted here.
The obtained current collector has a three-dimensional porous structure, and no granular substances exist, but the three-dimensional structure is broken incompletely.
example 4
the difference from example 1 is: (1) 1.4g of citric acid and 17.55g of sodium chloride were weighed, the mixture was dissolved in 100ml of deionized water and stirred magnetically for 4 hours to obtain a homogeneous solution. Pouring the uniformly mixed liquid into a culture dish, and then freezing the culture dish for 24 hours in a refrigerator at the temperature of-20 ℃; freeze-drying the frozen sample in a freeze-dryer under the following conditions: -50 ℃, 20Pa, lyophilization time 24 h. Grinding the freeze-dried sample to obtain precursor composite powder (the particle size of the powder is 100 meshes); putting 10g of the powder into a square boat, putting the square boat into a tubular furnace, introducing 500ccm argon for 15min to remove air, adjusting the temperature to 200ccm, heating to 750 ℃ at a heating rate of 10 ℃/min, preserving heat for 2h, quickly cooling to room temperature after heat preservation, putting the calcined powder into a 500ml beaker, adding 400ml of deionized water, magnetically stirring for 30min to completely dissolve sodium chloride in water, then carrying out suction filtration, repeatedly carrying out three times, putting the suction-filtered sample into a 70 ℃ vacuum oven, and drying for 3h to obtain the three-dimensional porous carbon loaded molybdenum disulfide composite material. The rest is the same as embodiment 1, and the description is omitted here.
The resulting current collector presents a three-dimensional porous structure, but according to XRD testing shows no MoS therein2Present, noted as 3 DC.
Claims (3)
1. A preparation method of a three-dimensional porous carbon loaded flaky molybdenum disulfide current collector for a lithium metal negative electrode comprises the following steps:
(1) Taking one or more of sucrose, glucose, citric acid and starch as a carbon source, ammonium molybdate as a molybdenum source, thiourea as a sulfur source, one or more of sodium sulfate, sodium chloride, sodium carbonate and sodium silicate as a template, and taking the molar ratio of molybdenum atoms in the molybdenum source, sulfur atoms in the sulfur source and carbon atoms in the carbon source as 1: (2-10): (50-500), adding a molybdenum source, a sulfur source, a carbon source and a salt template into deionized water for dissolving, and preparing a uniform and transparent precursor solution.
(2) Freeze-drying the precursor solution prepared in the last step to obtain dry solid powder, and grinding to obtain a mixed powder precursor;
(3) Placing the mixed powder precursor obtained in the last step into a tubular furnace hearth; heating to 500-750 ℃ at a heating rate of 1-10 ℃ in an inert gas atmosphere, preserving heat for a period of time, and then rapidly cooling to obtain a calcined product;
(4) Carrying out suction filtration on the calcined product obtained in the last step by using deionized water, removing NaCl, and drying to obtain a three-dimensional porous carbon loaded flaky molybdenum disulfide material;
(5) Mixing the three-dimensional porous carbon loaded flaky molybdenum disulfide material prepared in the step (4) with polyvinylidene fluoride (PVDF) by the ratio of 8: and (1) mixing the materials according to the mass ratio, adding a proper amount of N-methyl pyrrolidone (NMP) to prepare slurry, uniformly mixing the slurry, coating the slurry on a copper foil, and drying to obtain the three-dimensional porous carbon loaded flaky molybdenum disulfide composite current collector.
2. The method according to claim 1, wherein the cooling rate in the step (3) is 50-100 ℃/min on average.
3. A battery is assembled by using the three-dimensional porous carbon loaded flaky molybdenum disulfide composite current collector prepared in the claim 1, and a counter electrode is a lithium sheet.
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| CN111422906A (en) * | 2020-02-29 | 2020-07-17 | 合肥国轩高科动力能源有限公司 | Preparation method of silylene and molybdenum disulfide lithium battery cathode composite material |
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