CN110767889A - Preparation method of lithium-sulfur battery positive electrode material - Google Patents
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Abstract
The invention relates to a preparation method of a lithium-sulfur battery, wherein a layer of ZIF8 particles grows on a positive electrode material by taking a carbon nano tube and reduced graphene oxide as substrates, and then the positive electrode material is compounded with sulfur to be used as the positive electrode material for the lithium-sulfur battery. The composite material can solve the problem of poor sulfur conductivity, and the lithium polysulfide can be effectively adsorbed and converted by the aid of the ultrahigh specific surface area and the ZIF8, so that redox reaction in an electrode is promoted, the shuttle effect of polysulfide is inhibited, and the electrical property of a lithium sulfur battery is improved.
Description
Technical Field
The technical scheme of the invention relates to a preparation method of a lithium-sulfur battery anode material taking RGO and CNT as substrates, belonging to the field of material chemistry.
Background
Secondary batteries with high energy density have great significance and great value in the development of modern human society. With the rapid development of electric vehicles and other portable mobile devices, consumers urgently need a high energy density secondary battery having high energy density and good cycle performance to further meet the needs of efficient and convenient production and life.
Among a plurality of secondary battery systems, the lithium sulfur battery has outstanding advantages by taking elemental sulfur and metallic lithium as positive and negative active materials. In the using process of the battery, sulfur is subjected to oxidation-reduction reaction between 0 valence and-2 valence, and the sulfur anode has very high specific capacity due to multi-electron conversion reaction, wherein the theoretical specific capacity is up to 1672mAh/g, which is far higher than the specific capacity of the anode material of the traditional lithium ion battery. Meanwhile, the sulfur is abundant in nature and low in price, so that the lithium-sulfur battery is expected to become a cheap large-scale energy storage technology. Compared with other high-energy-density battery systems such as a lithium air battery and the like, the lithium sulfur battery is a closed system, so that the pollution of the battery system exposed to air is avoided, and the potential explosion hazard is lower. Therefore, the lithium-sulfur battery is expected to become a next-generation high-energy-density secondary battery that is widely used.
However, there are many problems to be solved in the application of lithium sulfur batteries. Firstly, the anode material of the lithium-sulfur battery is elemental sulfur, the conductivity of the elemental sulfur is extremely low, and the reaction between solids is difficult to carry out at normal temperature, so that the anode material needs to be compounded with a conductive material to improve the overall conductivity of the material, and secondly, an electrolyte system capable of dissolving polysulfide is used, and the solid-phase conversion of an active substance is controlled by using a soluble intermediate polysulfide, so that the electrode material can fully react. However, the solubility of polysulfides poses new problems. Polysulfide dissolves in the electrolyte and can penetrate the separator, and oxidation-reduction reaction occurs at the lithium negative electrode, so that the shuttle effect is caused. The shuttle effect of polysulfide not only aggravates the rapid attenuation of battery capacity, but also causes the problems of low charging and discharging efficiency, self-discharging and the like. Meanwhile, the repeated deposition of sulfur also causes drastic changes in the structure of the positive electrode, and the reaction of polysulfide at the negative electrode interface also causes irreversible deposition of active materials and destruction of interface stability.
In order to solve the above problems and promote the practical development of the system, a large amount of research and inventions have been optimized for the positive electrode, electrolyte and separator of the battery. Wherein the improvement and preparation of the battery anode material are developed most rapidly and have outstanding advantages. Polysulfide is generated mainly at the positive collector, and by compounding sulfur with a material capable of binding polysulfide, not only the conductivity of the positive electrode material can be improved, but also polysulfide can be adsorbed and converted more rapidly and efficiently. The commonly used composite material mainly comprises a carbon-based composite material and a metal oxide material, and after the carbon-based composite material and the metal oxide material are compounded with active substance sulfur, the diffusion of sulfide is effectively inhibited through the adsorption or blocking effect, so that the specific capacity of the battery is improved, and the cycle performance is improved to a certain extent. These processes are still limited in their ability to convert and regulate polysulfides.
In recent years, various metal organic frameworks are applied to lithium sulfur batteries due to high specific surface areas and adsorption effects on polysulfides, and are used for inhibiting shuttle effects of polysulfides, but most of metal organic frameworks have low electrical conductivity, cannot improve the problem that the electrical conductivity of a positive electrode material is poor after being compounded with sulfur, and are not ideal for improving the specific capacity and the cycle performance of the lithium sulfur batteries. Based on the above analysis, if the conductive carbon-based material and the metal-organic framework can be combined and supported on the conductive carbon-based material, the conventional problems can be effectively solved. The metal organic framework loaded on the conductive carbon-based material can effectively adsorb polysulfide and promote electrochemical reaction of the polysulfide, and meanwhile, the carbon-based material can effectively improve the conductivity of the electrode material, so that the conversion, reaction and deposition of the active substance of the battery are greatly optimized, the coulombic efficiency, specific capacity and cycling stability are greatly improved, and the high-capacity and high-rate charge and discharge cycle capability is also good.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a positive electrode material for a lithium-sulfur battery, which is prepared by growing a layer of ZIF8 particles on a substrate of a carbon nano tube and reduced graphene oxide and compounding the particles with sulfur, and a preparation method thereof, and aims to solve the problems of high load capacity and high rate cycle of the conventional lithium-sulfur battery. The prepared RGO-CNT/ZIF8 composite material is combined with sulfur to be used as a positive electrode material of a lithium-sulfur battery, so that the problem of poor sulfur conductivity can be solved, lithium polysulfide can be effectively adsorbed and converted by the aid of the ultrahigh specific surface area and the ZIF8, redox reaction in an electrode is promoted, and the shuttle effect of polysulfide is restrained.
A preparation method of a lithium-sulfur battery positive electrode material specifically comprises the following steps:
the first step is as follows: preparation of RGO-CNT/ZnO Material:
a certain amount of Zn (CH)3COO)2·H2Adding O into methanol, heating to 65 deg.C and stirring to dissolve completely to obtain Zn (CH)3COO)2And (3) solution. Adding a certain amount of KOH into methanol, heating to 65 ℃ and stirring until the KOH is completely dissolved to obtain a KOH solution. Adding certain amount of CNT and RGO into methanol, recording as CNT/RGO solution, ultrasonic treating for 20-30min, and adding into the Zn (CH)3COO)2And continuously stirring the solution at 65 ℃ for 20min, then dripping a KOH solution into the mixed solution by using a dropper, continuously and quickly stirring, reacting for 2h, centrifugally collecting precipitates, and drying to obtain the RGO-CNT/ZnO material.
Further, Zn (CH) in the first step3COO)2Zn (CH) in solution3COO)2·H2The molar concentration of O is 0.035 mol/L; the molar concentration of the KOH mass in the KOH solution is 0.106 mol/L;
further, the mass-to-volume ratio of CNT to methanol in the first step is 10: 3g/L, the mass volume ratio of RGO to methanol is 10: 3 g/L.
Further, the Zn (CH)3COO)2The volume ratio of the solution, KOH solution, and CNT/RGO solution was 5:4: 3.
The second step is that: preparation of RGO-CNT/ZIF8 composite:
adding 2-methylimidazole into methanol, heating the methanol on a heating plate to 50 ℃ to completely dissolve the 2-methylimidazole to obtain a 2-methylimidazole solution; adding the RGO-CNT/ZnO material prepared in the first step into methanol, and performing ultrasonic treatment for 30min to obtain an RGO-CNT/ZnO solution; adding the RGO-CNT/ZnO solution into the 2-methylimidazole solution, stirring at 50 ℃ for 10min-30min, centrifuging to collect precipitates, centrifugally washing for 5 times by using anhydrous methanol, and drying at 60 ℃ overnight to obtain the RGO-CNT/ZIF8 composite material.
Further, the mass volume ratio of the 2-methylimidazole to the methanol in the 2-methylimidazole solution in the second step is 20.5-82:1 g/L; the mass volume ratio of the RGO-CNT/ZnO material to the methanol in the RGO-CNT/ZnO solution is 10:1 g/L;
further, the volume ratio of the 2-methylimidazole solution to the RGO-CNT/ZnO solution is 5: 1.
The third step: preparation of RGO-CNT/ZIF8-S cathode material
Mixing sublimed sulfur and an RGO-CNT/ZIF8 composite material according to a mass ratio of 1:3, grinding for 30min, and dropwise adding 2-3 drops of CS into the mixed powder2Continuing to grind to CS2The whole solution was volatilized and the operation was repeated 20 times. And (3) placing the mixed material in a 25ml stainless steel reaction kettle, filling argon into the kettle, heating to 155 ℃, and preserving heat for 12 hours.
The preparation method of the RGO-CNT/ZIF8 composite material for the lithium-sulfur battery is commercially available.
The invention has the following beneficial effects:
(1) in the design process of the invention, the structural problem of the sulfur-based positive electrode material in the lithium-sulfur battery is fully considered, and the functional material which can inhibit the shuttle effect of polysulfide grows on the RGO-CNT serving as the substrate is innovatively provided, and is compositely treated with sulfur to serve as the positive electrode material of the lithium-sulfur battery, so that the electrochemical performance of the lithium-sulfur battery is greatly improved.
(2) The RGO-CNT is used as a material, so that the conductivity of the material can be improved, the transmission efficiency of electrons and ions in the charge and discharge process of the battery is improved, the redox reaction of the lithium-sulfur battery in the charge and discharge process is promoted, and the cycle and rate performance of the battery are improved. The higher specific surface area can also greatly improve the loading capacity of the functional material, thereby strengthening the inhibiting effect on the 'shuttle effect' of polysulfide.
Drawings
FIG. 1 is a partial scanning electron micrograph of the RGO-CNT/ZIF8 composite prepared in example 1.
FIG. 2 is a graph of the cycling performance of button cells made from the RGO-CNT/ZIF8 composite material made in example 1 mixed with sulfur as the positive electrode material.
Example 1:
the first step is as follows: preparation of GO-CNT/ZnO materials:
0.3864g of Zn (CH) were weighed out3COO)2·H2Adding O into 50ml methanol, placing on a heating plate, stirring at 65 deg.C to completely dissolve to obtain Zn (CH)3COO)2·H2And (4) O solution. 0.2384g of KOH were weighed into 40ml of methanol, and placed on a heating plate and stirred at 65 ℃ until completely dissolved to obtain a KOH solution. Weighing 0.1g CNT and 0.1g CGO, adding into 30ml methanol, ultrasonic treating for 20-30min, adding into Zn (CH)3COO)2·H2O solution, stirred at 65 ℃ for 20 min. And dripping a KOH solution into the mixed solution by using a dropper, quickly stirring, reacting for 2 hours, centrifugally collecting precipitates, and drying to obtain the GO-CNT/ZnO material.
The second step is that: preparation of RGO-CNT/ZIF8 composite:
2.05g of 2-methylimidazole is weighed and added into 50ml of methanol, and the mixture is placed on a heating plate and heated to 50 ℃ until the mixture is completely dissolved to obtain a 2-methylimidazole solution; weighing 0.1g of RGO-CNT/ZnO material prepared in the first step, adding into 10ml of anhydrous methanol, and carrying out ultrasonic treatment for 30min to obtain an RGO-CNT/ZnO solution; adding the RGO-CNT/ZnO solution into the 2-methylimidazole solution, stirring for 20min at 50 ℃, centrifuging to collect precipitates, centrifugally washing for 5 times by using anhydrous methanol, and drying at 60 ℃ overnight to obtain the RGO-CNT/ZIF8 composite material.
The third step: preparation of RGO-CNT/ZIF8-S cathode material
Mixing sublimed sulfur and an RGO-CNT/ZIF8 composite material according to a mass ratio of 1:3, grinding for 30min, and dropwise adding 2-3 drops of CS into the mixed powder2Continuing to grind to CS2The whole solution was volatilized and the operation was repeated 20 times. And (3) placing the mixed material in a 25ml stainless steel reaction kettle, filling argon into the kettle, heating to 155 ℃, and preserving heat for 12 hours.
As can be seen from fig. 1, a layer of ZIF8 particles was uniformly grown on the carbon nanotubes, and no agglomeration occurred. The structure can enable the material to have a larger specific surface knot, and can better inhibit the shuttle effect of polysulfide.
Fig. 2 shows that the battery has good cycle performance and low capacity attenuation, and the specific capacity can still reach 820mAh/g after 80 cycles.
Example 2:
the first step is as follows: preparation of GO-CNT/ZnO materials:
0.3864g of Zn (CH) were weighed out3COO)2·H2Adding O into 50ml methanol, placing on a heating plate, stirring at 65 deg.C to completely dissolve to obtain Zn (CH)3COO)2·H2And (4) O solution. 0.2384g of KOH were weighed into 40ml of methanol, and placed on a heating plate and stirred at 65 ℃ until completely dissolved to obtain a KOH solution. Weighing 0.1g CNT and 0.1g CGO, adding into 30ml methanol, ultrasonic treating for 20-30min, adding into Zn (CH)3COO)2·H2O solution, stirred at 65 ℃ for 20 min. And dripping a KOH solution into the mixed solution by using a dropper, quickly stirring, reacting for 2 hours, centrifugally collecting precipitates, and drying to obtain the GO-CNT/ZnO material.
The second step is that: preparation of RGO-CNT/ZIF8 composite:
weighing 1.025g of 2-methylimidazole, adding the 2-methylimidazole into 50ml of methanol, and heating the mixture on a heating plate to 50 ℃ until the 2-methylimidazole is completely dissolved to obtain a 2-methylimidazole solution; weighing 0.1g of RGO-CNT/ZnO material prepared in the first step, adding into 10ml of anhydrous methanol, and carrying out ultrasonic treatment for 30min to obtain an RGO-CNT/ZnO solution; the RGO-CNT/ZnO solution was added to the 2-methylimidazole solution and stirred at 50 ℃ for 10 min. Centrifuging to collect precipitate, centrifuging and washing with anhydrous methanol for 5 times, and drying at 60 deg.C overnight to obtain RGO-CNT/ZIF8 composite material.
The third step: preparation of RGO-CNT/ZIF8-S cathode material
Mixing sublimed sulfur and an RGO-CNT/ZIF8 composite material according to a mass ratio of 1:3, grinding for 30min, and dropwise adding 2-3 drops of CS into the mixed powder2Continuing to grind to CS2The whole solution was volatilized and the operation was repeated 20 times. And (3) placing the mixed material in a 25ml stainless steel reaction kettle, filling argon into the kettle, heating to 155 ℃, and preserving heat for 12 hours.
Example 3:
the first step is as follows: preparation of GO-CNT/ZnO materials:
weigh 0.3864g Zn(CH3COO)2·H2Adding O into 50ml methanol, placing on a heating plate, stirring at 65 deg.C to completely dissolve to obtain Zn (CH)3COO)2·H2And (4) O solution. 0.2384g of KOH were weighed into 40ml of methanol, and placed on a heating plate and stirred at 65 ℃ until completely dissolved to obtain a KOH solution. Weighing 0.1g CNT and 0.1g CGO, adding into 30ml methanol, ultrasonic treating for 20-30min, adding into Zn (CH)3COO)2·H2O solution, stirred at 65 ℃ for 20 min. And dripping a KOH solution into the mixed solution by using a dropper, quickly stirring, reacting for 2 hours, centrifugally collecting precipitates, and drying to obtain the GO-CNT/ZnO material.
The second step is that: preparation of RGO-CNT/ZIF8 composite:
weighing 2-methylimidazole 4.10g, adding into 50ml methanol, heating to 50 ℃ on a heating plate until completely dissolving to obtain 2-methylimidazole solution; weighing 0.1g of RGO-CNT/ZnO material prepared in the first step, adding into 10ml of anhydrous methanol, and carrying out ultrasonic treatment for 30min to obtain an RGO-CNT/ZnO solution; adding the RGO-CNT/ZnO solution into the 2-methylimidazole solution, stirring for 30min at 50 ℃, centrifuging to collect precipitates, centrifugally washing for 5 times by using anhydrous methanol, and drying at 60 ℃ overnight to obtain the RGO-CNT/ZIF8 composite material.
The third step: preparation of RGO-CNT/ZIF8-S cathode material
Mixing sublimed sulfur and an RGO-CNT/ZIF8 composite material according to a mass ratio of 1:3, grinding for 30min, and dropwise adding 2-3 drops of CS into the mixed powder2Continuing to grind to CS2The whole solution was volatilized and the operation was repeated 20 times. And (3) placing the mixed material in a 25ml stainless steel reaction kettle, filling argon into the kettle, heating to 155 ℃, and preserving heat for 12 hours.
Claims (6)
1. A preparation method of a lithium-sulfur battery positive electrode material comprises the following steps:
the first step is as follows: preparation of RGO-CNT/ZnO Material:
a certain amount of Zn (CH)3COO)2·H2Adding O into methanol, heating to 65 deg.C and stirring to dissolve completely to obtain Zn (CH)3COO)2A solution; adding a certain amount of KOH into methanol, heating to 65 deg.CAnd stirring until the KOH solution is completely dissolved to obtain a KOH solution; adding certain amount of CNT and RGO into methanol, recording as CNT/RGO solution, ultrasonic treating for 20-30min, and adding into the Zn (CH)3COO)2Continuously stirring the solution at 65 ℃ for 20min, then dropwise adding the KOH solution into the mixed solution by using a dropper, continuously and quickly stirring, centrifugally collecting precipitates after reacting for 2h, and drying to obtain an RGO-CNT/ZnO material;
the second step is that: preparation of RGO-CNT/ZIF8 composite:
adding 2-methylimidazole into methanol, heating to 50 ℃ and completely dissolving to obtain a 2-methylimidazole solution;
adding the RGO-CNT/ZnO material prepared in the first step into methanol, and performing ultrasonic treatment for 30min to obtain an RGO-CNT/ZnO solution; adding the RGO-CNT/ZnO solution into the 2-methylimidazole solution, stirring for 10min-30min at 50 ℃, centrifuging to collect precipitates, centrifugally washing for 5 times by using anhydrous methanol, and drying overnight at 60 ℃ to obtain the RGO-CNT/ZIF8 composite material.
The third step: preparation of RGO-CNT/ZIF8-S cathode material
Mixing sublimed sulfur and an RGO-CNT/ZIF8 composite material according to a mass ratio of 1:3, grinding for 30min, and dropwise adding 2-3 drops of CS into the mixed powder2Continuing to grind to CS2The whole solution was volatilized and the operation was repeated 20 times. And (3) placing the mixed material in a 25ml stainless steel reaction kettle, filling argon into the kettle, heating to 155 ℃, and preserving heat for 12 hours.
2. The method of claim 1, wherein: zn (CH) in the first step3COO)2Zn (CH) in solution3COO)2·H2The molar concentration of O is 0.035 mol/L; the molar concentration of the KOH mass in the KOH solution is 0.106 mol/L.
3. The method of claim 1, wherein: in the CNT/RGO solution, the mass-to-volume ratio of CNT to methanol is 10: 3g/L, the mass volume ratio of RGO to methanol is 10: 3 g/L.
4. The production method according to any one of claims 1 to 3, characterized in that: the Zn (CH)3COO)2The volume ratio of the solution, KOH solution, and CNT/RGO solution was 5:4: 3.
5. The method of claim 1, wherein: in the second step, the mass volume ratio of the 2-methylimidazole to the methanol in the 2-methylimidazole solution is 20.5-82:1 g/L; the mass volume ratio of the RGO-CNT/ZnO material to the methanol in the RGO-CNT/ZnO solution is 10:1 g/L.
6. The method of claim 5, wherein: the volume ratio of the 2-methylimidazole solution to the RGO-CNT/ZnO solution is 5: 1.
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| CN114783782B (en) * | 2022-04-25 | 2023-12-22 | 武汉大学 | Three-dimensional graphene-metal organic frame electrode for 3D printing, and preparation method and application thereof |
| CN115911308A (en) * | 2022-11-09 | 2023-04-04 | 西南石油大学 | Composite sulfur positive electrode material and preparation method thereof, and composite sulfur positive electrode and preparation method thereof |
| CN115911308B (en) * | 2022-11-09 | 2023-09-22 | 西南石油大学 | Composite sulfur positive electrode material and preparation method thereof, and composite sulfur positive electrode and preparation method thereof |
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