CN112490420B - Maltose-derived carbon/lithium sulfide composite electrode material and preparation method and application thereof - Google Patents
Maltose-derived carbon/lithium sulfide composite electrode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a maltose derived carbon/lithium sulfide composite material and a preparation method and application thereof, wherein the preparation method comprises the following steps: obtaining maltose; and compounding the maltose-derived carbon with the lithium sulfide nanoparticles, and carbonizing at high temperature for 3h, 4h and 5h to synthesize the maltose-derived carbon-based lithium sulfide three-dimensional porous composite material. The composite material has the characteristics of high specific surface area, high cycling stability, rate capability, coulombic efficiency and the like, and is particularly suitable for serving as a lithium-sulfur battery positive electrode material.
Description
Technical Field
The invention relates to the technical field of lithium-sulfur battery positive electrode materials, in particular to a maltose-derived carbon/lithium sulfide composite electrode material and a preparation method and application thereof.
Background
So far, lithium ion batteries are still the most widely commercialized batteries. However, with the development and progress of society, the low energy density (200-250 Wh/kg) can not meet the requirement of society for high energy density batteries. Therefore, new high energy density battery systems are urgently sought. Among the numerous battery systems, lithium sulfur batteries are of most interest because they have a high energy density (2600Wh/kg) and a volume density (2800Wh/L), twice that of commercial lithium ion batteries. The sulfur anode has a theoretical capacity of 1675mAh/g, is low in price and environment-friendly, and is also concerned. However, lithium sulfur batteries have some intrinsic defects that prevent their further development: 1) the shuttling effect of the intermediate (polysulfide) leads to the generation of irreversible capacity and reduces coulombic efficiency and greatly limits its cyclic stability. 2) The dendrite problem of lithium metal causes the separator to be broken, and the safety performance of the battery is reduced. Therefore, the lithiated lithium sulfide positive electrode is produced and can be matched with negative electrodes such as Si, Al and graphite, so that lithium metal is avoided, the problem of lithium dendrite is solved on the source, and the safety performance of the battery is greatly improved. However, the shuttling effect of polysulfides is still not addressed by the use of lithium sulfide as the positive electrode, and the insulating properties of lithium sulfide further limit its research.
In view of the above problems, researchers mainly adopt the following strategies to modify lithium sulfide electrodes: 1) compounding lithium sulfide with high-conductivity substance such as carbon material to improve electronic conductivity of active material; 2) the compound is compounded with polar compounds such as oxides, carbides, sulfides and the like, and the adsorption effect is generated on soluble polysulfide, so that the shuttle effect is inhibited; 3) and a porous structure is constructed, the reaction area of the sulfide active substance and the electrolyte is increased, and the utilization rate of the sulfide active substance is increased, so that the electrochemical performance of the sulfide active substance is improved. The method is an effective modification method by compounding lithium sulfide and a high-conductivity porous carbon material. Therefore, the invention of the porous carbon material which is suitable for large-scale production and has high conductivity is very necessary and is a better way for improving the electrochemical performance of the lithium sulfide positive electrode.
Disclosure of Invention
Aiming at the problems in the background art, the invention aims to provide a maltose-derived carbon/lithium sulfide composite electrode material and a preparation method and application thereof, the maltose-derived carbon/lithium sulfide composite electrode material with high capacity is synthesized, and the electronic conductivity of the electrode is improved, the shuttle problem of polysulfide is relieved and the electrochemical performance of the electrode is improved by constructing a three-dimensional cross-linked porous conductive substrate.
A preparation method of a maltose-derived carbon/lithium sulfide composite electrode material comprises the following steps:
(1) preparing maltose;
(2) preparing a lithium sulfate solution, pouring the lithium sulfate solution into maltose, ultrasonically stirring, and then freeze-drying for 12-48h by using a freeze dryer to obtain a precursor;
(3) transferring the precursor to a tubular furnace, carrying out preheating treatment at the temperature of 500-700 ℃ in argon for 3-6 h, then sintering the precursor into a phase at the temperature of 700-900 ℃ for 3-6 h, and cooling to obtain the maltose-derived carbon/lithium sulfide composite material;
the following are preferred technical schemes of the invention:
in the step (1), the preparation of maltose specifically comprises:
cleaning Oryza Glutinosa, adding into a pan, stewing, mixing with chopped fructus Hordei Germinatus, fermenting for 4-6 hr until the juice is converted, filtering out the juice, heating and decocting to obtain paste, and cooling to obtain amber sugar block.
In the step (2), the lithium sulfate solution is prepared by adopting lithium sulfate and deionized water.
The mass ratio of the lithium sulfate to the deionized water to the maltose is 1: 1.5-2.5: 3 to 5. Most preferably, the mass ratio of the lithium sulfate, the deionized water and the maltose is 1: 2: 4.
the lithium sulfate solution is poured into maltose and stirred ultrasonically for 20-40min, preferably 30 min.
Followed by lyophilization with a lyophilizer for 18-30h, most preferably 24 h.
In the step (3), the preheating treatment is performed at 550-650 ℃ for 3-6 h in argon, and most preferably, the preheating treatment is performed at 600 ℃ for 4h in argon.
Then sintering the mixture into a phase at 800-900 ℃ for 3-6 h, most preferably sintering the mixture into a phase at 850 ℃ for 3-5 h.
Most preferably, the preparation method of the maltose-derived carbon/lithium sulfide composite electrode material comprises the following steps:
(1) cleaning glutinous rice, stewing in pot, mixing with chopped fructus Hordei Germinatus, and fermenting for 4-6 hr until juice is obtained. Filtering to obtain juice, decocting at high temperature to obtain paste, and cooling to obtain amber-like sugar block.
(2) Preparing a lithium sulfate solution, pouring the solution into maltose, ultrasonically stirring for 30min, and then freeze-drying for 24h by using a freeze dryer.
(3) Preheating the precursor obtained by freeze drying at 600 ℃ for 4h in argon, transferring the precursor into a tubular furnace at 850 ℃ to sinter the precursor into a phase for 4h, wherein the heating rate is 5 ℃/min, and cooling to obtain the maltose-derived carbon/lithium sulfide composite material.
A maltose-derived carbon/lithium sulfide composite material comprising a three-dimensionally crosslinked porous maltose-derived carbon and an active material lithium sulfide nanoparticle. The maltose-derived carbon/lithium sulfide composite electrode material takes three-dimensional flaky cross-linked maltose-derived carbon as a main substrate, lithium sulfide nano particles grow through in-situ carbothermic reaction, a large number of mesoporous structures are generated to form a multi-level structure, the thickness of the maltose-derived carbon sheet layer is 200-500nm, the size of the lithium sulfide nano particles is 15-30nm, and the size of the generated mesoporous is 20-40 nm.
The high-capacity maltose-derived carbon/lithium sulfide composite electrode material can be used for improving the electronic conductivity of an electrode and inhibiting the shuttle effect of a lithium-sulfur battery, takes the high-conductivity maltose-derived carbon as a carrier, loads lithium sulfide nano particles, constructs a multi-level pore channel structure, synergistically optimizes the electrochemical performance of a lithium sulfide anode, and is very suitable for being used as an anode material of the lithium-sulfur battery.
Compared with the prior art, the invention has the following advantages and outstanding effects:
according to the invention, the maltose-derived carbon/lithium sulfide composite electrode material adopts high-conductivity maltose-derived carbon as a main carrier, has a three-dimensional cross-linked porous structure, improves the electronic conductivity of the electrode, and strengthens the physical adsorption of polysulfide, thereby improving the electrochemical dynamics and reducing the irreversible capacity; meanwhile, in the in-situ formation process of the lithium sulfide nanoparticles, a large number of mesoporous channels are obtained, a multi-level porous structure is constructed, the specific surface area of the carrier and the contact area of the electrolyte are increased, and therefore the utilization rate of the active substance lithium sulfide is improved. The composite positive electrode improves the rate capability and the cycle performance of lithium sulfide, and is beneficial to promoting the development of a lithium-sulfur positive electrode with high energy density and high stability.
Drawings
FIG. 1 is a scanning electron micrograph of a maltose-derived carbon/lithium sulfide composite material prepared in example 3.
FIG. 2 is a transmission electron micrograph of the maltose-derived carbon/lithium sulfide composite material prepared in example 3, with inset electron diffraction patterns.
Fig. 3 is a transmission electron microscope image and an element distribution spectrum of the maltose-derived carbon/lithium sulfide composite material prepared in example 3, wherein in fig. 3, a is a transmission electron microscope image of the composite material, b is a total distribution spectrum of each element in the composite material, C is a distribution spectrum of an S element in the composite material, and d is a distribution spectrum of a C element in the composite material.
Detailed Description
The present invention will be described in detail with reference to examples, but the present invention is not limited thereto.
(1) Cleaning glutinous rice, stewing in pot, mixing with chopped fructus Hordei Germinatus, and fermenting for 4-6 hr until juice is obtained. Filtering to obtain juice, decocting at high temperature to obtain paste, and cooling to obtain amber-like sugar block.
(2) Preparing a lithium sulfate solution by adopting lithium sulfate and deionized water, wherein the mass ratio of the lithium sulfate to the deionized water to maltose is 1: 2: 4, the solution was poured into maltose and stirred ultrasonically for 30min, followed by freeze-drying for 24h with a freeze-dryer.
(3) Preheating the precursor obtained by freeze drying at 600 ℃ for 4h in argon, transferring the precursor into a tubular furnace at 850 ℃ to sinter the precursor into a phase for 4h, wherein the heating rate is 5 ℃/min, and cooling to obtain the maltose-derived carbon/lithium sulfide composite material.
Example 1
Cleaning glutinous rice, stewing in pot, mixing with chopped fructus Hordei Germinatus, and fermenting for 4-6 hr until juice is obtained. Filtering to obtain juice, decocting at high temperature to obtain paste, and cooling to obtain amber-like sugar block. Preparing a lithium sulfate solution by adopting lithium sulfate and deionized water, wherein the mass ratio of the lithium sulfate to the deionized water to maltose is 1: 2: 4, the solution was poured into maltose and stirred ultrasonically for 30min, followed by freeze-drying for 24h with a freeze-dryer. Preheating the precursor obtained by freeze drying at 600 ℃ for 4h in argon, transferring the precursor into a tubular furnace at 850 ℃ to sinter the precursor into a phase for 3h, wherein the heating rate is 5 ℃/min, and cooling to obtain the maltose-derived carbon/lithium sulfide composite material.
Example 2
Cleaning glutinous rice, stewing in pot, mixing with chopped fructus Hordei Germinatus, and fermenting for 4-6 hr until juice is obtained. Filtering to obtain juice, decocting at high temperature to obtain paste, and cooling to obtain amber-like sugar block. Preparing a lithium sulfate solution by adopting lithium sulfate and deionized water, wherein the mass ratio of the lithium sulfate to the deionized water to maltose is 1: 2: 4, the solution was poured into maltose and stirred ultrasonically for 30min, followed by freeze-drying for 24h with a freeze-dryer. Preheating the precursor obtained by freeze drying at 600 ℃ for 4h in argon, transferring the precursor into a tubular furnace at 850 ℃ to sinter the precursor into a phase for 5h, wherein the heating rate is 5 ℃/min, and cooling to obtain the maltose-derived carbon/lithium sulfide composite material.
Example 3
Cleaning glutinous rice, stewing in pot, mixing with chopped fructus Hordei Germinatus, and fermenting for 4-6 hr until juice is obtained. Filtering to obtain juice, decocting at high temperature to obtain paste, and cooling to obtain amber-like sugar block. Preparing a lithium sulfate solution by adopting lithium sulfate and deionized water, wherein the mass ratio of the lithium sulfate to the deionized water to maltose is 1: 2: 4, the solution was poured into maltose and stirred ultrasonically for 30min, followed by freeze-drying for 24h with a freeze-dryer. Preheating the precursor obtained by freeze drying at 600 ℃ for 4h in argon, transferring the precursor into a tubular furnace at 850 ℃ to sinter the precursor into a phase for 4h, wherein the heating rate is 5 ℃/min, and cooling to obtain the maltose-derived carbon/lithium sulfide composite material.
FIG. 1 is a scanning electron micrograph of a maltose-derived carbon/lithium sulfide composite material prepared in example 3. FIG. 2 is a transmission electron micrograph of the maltose-derived carbon/lithium sulfide composite material prepared in example 3, with inset electron diffraction patterns. Fig. 3 is a transmission electron microscope image and an element distribution spectrum of the maltose-derived carbon/lithium sulfide composite material prepared in example 3, wherein in fig. 3, a is a transmission electron microscope image of the composite material, b is a total distribution spectrum of each element in the composite material, C is a distribution spectrum of an S element in the composite material, and d is a distribution spectrum of a C element in the composite material. Fig. 1, 2 and 3 show maltose-derived carbon/lithium sulfide composite materials comprising three-dimensionally crosslinked porous maltose-derived carbon and active material lithium sulfide nanoparticles. The maltose-derived carbon/lithium sulfide composite electrode material takes three-dimensional flaky cross-linked maltose-derived carbon as a main substrate, lithium sulfide nano particles grow in a hot and small mode through in-situ carbon heating, a large number of mesoporous structures are generated to form a multi-level structure, the thickness of the maltose-derived carbon sheet layer is 200-500nm, the size of the lithium sulfide nano particles is 15-30nm, and the size of generated mesopores is 20-40 nm.
Performance testing
The maltose-derived carbon/lithium sulfide composite materials prepared in the above examples 1 to 3 were assembled into a half cell using a lithium metal wafer as a counter electrode for electrochemical test, and 1M LiTFSI + DOL/DME (1:1) was used as an electrolyte. And sequentially adding the positive pole piece, the electrolyte, the diaphragm and the lithium piece into the positive shell for battery assembly, compacting and sealing the battery in a full-automatic packaging machine after the battery is assembled, standing for 24 hours, and performing electrochemical test by adopting a blue electricity and electrochemical workstation. The electrochemical tests are carried out under the constant temperature condition of 25 ℃, and mainly comprise constant current charge and discharge tests and cyclic voltammetry tests. In the constant current charge and discharge test, indexes such as multiplying power performance, cycle performance, polarization voltage and the like are mainly included. The test voltage range of the battery is 1.7-2.8V relative to (Li/Li)+) The multiplying power test current is 0.1C,0.2C,0.5C,1C,2C and 5C, and the cycle test current is 0.5C.
The performance test results are as follows:
the maltose-derived carbon/lithium sulfide composite electrodes of example 1, example 2 and example 3 had initial discharge capacities of 1032mAh/g, 1152mAh/g and 1315mAh/g, respectively, at 0.5C charge-discharge cycles. In addition, after 500 cycles of circulation, the discharge specific capacity retention rate of the three electrodes is up to 60%, and the coulombic efficiency is up to more than 95%. It can be seen that the battery formed by the maltose-derived carbon/lithium sulfide composite electrode prepared as described above has high discharge capacity and good cycle stability. Better results were also obtained in the rate performance tests of the maltose-derived carbon/lithium sulfide composite electrodes of example 1, example 2 and example 3, and the specific discharge capacities were 568mAh/g, 672mAh/g and 829mAh/g, respectively, at a current density of 2C. Therefore, the maltose-derived carbon/lithium sulfide composite material prepared by the method has excellent performance during large-current charging and discharging.
The electrode of the maltose-derived carbon/lithium sulfide composite material is of a porous structure, so that the loading capacity of active substance sulfur is increased, and the contact area between the surface of the electrode and electrolyte is increased; secondly, the maltose-derived carbon has higher electronic conductivity, so that the conductivity of the electrode can be greatly improved, and the interface reaction is accelerated; the maltose-derived carbon has in-situ doped phosphorus and nitrogen elements, so that the conductivity of the electrode can be further improved, and electron/ion transmission is promoted; meanwhile, in the in-situ formation process of the lithium sulfide nanoparticles, a large number of mesoporous channels are obtained, a multi-level porous structure is constructed, the specific surface area of the carrier and the contact area of the electrolyte are increased, the utilization rate of the active substance lithium sulfide is improved, and the electrochemical performance of the electrode is improved.
Therefore, the maltose-derived carbon/lithium sulfide composite material electrode has the characteristics of high cycle stability, high rate performance, coulombic efficiency and the like, and is expected to become a lithium-sulfur battery positive electrode material with high energy density for commercial application.
Claims (6)
1. A preparation method of a maltose-derived carbon/lithium sulfide composite electrode material is characterized by comprising the following steps:
(1) the preparation method of the maltose specifically comprises the following steps:
cleaning glutinous rice, stewing in a pan, mixing with chopped fructus Hordei Germinatus, fermenting for 4-6 hr until the juice is converted, filtering, heating and decocting to obtain paste, and cooling to obtain amber sugar block to obtain maltose;
(2) preparing a lithium sulfate solution, pouring the lithium sulfate solution into maltose, ultrasonically stirring, and then freeze-drying for 12-48h by using a freeze dryer to obtain a precursor;
the lithium sulfate solution is prepared by lithium sulfate and deionized water;
the mass ratio of the lithium sulfate to the deionized water to the maltose is 1: 1.5-2.5: 3-5;
pouring the lithium sulfate solution into maltose, and ultrasonically stirring for 20-40 min;
(3) and transferring the precursor to a tubular furnace, carrying out preheating treatment at the temperature of 500-700 ℃ in argon for 3-6 h, then sintering the precursor into a phase at the temperature of 700-900 ℃ for 3-6 h, and cooling to obtain the maltose-derived carbon/lithium sulfide composite material.
2. The method for preparing a maltose-derived carbon/lithium sulfide composite electrode material as claimed in claim 1, wherein in the step (2), the maltose-derived carbon/lithium sulfide composite electrode material is freeze-dried for 18-30h by a freeze-dryer.
3. The method for preparing a maltose-derived carbon/lithium sulfide composite electrode material as claimed in claim 1, wherein in the step (3), the preheating treatment is performed at 550-650 ℃ for 3-6 h in argon.
4. The method for preparing a maltose-derived carbon/lithium sulfide composite electrode material as claimed in claim 1, wherein in the step (3), the maltose-derived carbon/lithium sulfide composite electrode material is sintered into a phase at 800-900 ℃ for 3-6 h.
5. The maltose-derived carbon/lithium sulfide composite electrode material prepared by the preparation method according to any one of claims 1 to 4, characterized by comprising three-dimensionally crosslinked porous maltose-derived carbon and active material lithium sulfide nanoparticles.
6. Use of the maltose-derived carbon/lithium sulfide composite electrode material according to claim 5 as a lithium sulfur battery positive electrode material.
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| CN103829012A (en) * | 2014-02-24 | 2014-06-04 | 郎溪县睿智生产力促进中心有限公司 | Preparation method of maltose |
| CN106099069A (en) * | 2016-08-15 | 2016-11-09 | 华南理工大学 | A kind of sodium-ion battery negative pole SnS/C composite and preparation method thereof |
| CN109360953A (en) * | 2018-09-28 | 2019-02-19 | 天津大学 | A kind of method synthesizing vulcanization lithium/carbon composite material and the lithium-sulfur cell using the material |
| CN110137462A (en) * | 2019-05-10 | 2019-08-16 | 浙江大学 | Preparation method for aluminium/lithium sulphide battery vulcanization lithium/carbon composite material |
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| FR3071361B1 (en) * | 2017-09-15 | 2019-09-13 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | PROCESS FOR PRODUCING LITHIUM-SULFUR ACCUMULATOR ELECTRODE USING LI2S AS ACTIVE MATERIAL |
| CN111628150B (en) * | 2020-06-04 | 2021-10-08 | 合肥工业大学 | Carbon-coated lithium sulfide composite electrode for lithium-sulfur battery and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103829012A (en) * | 2014-02-24 | 2014-06-04 | 郎溪县睿智生产力促进中心有限公司 | Preparation method of maltose |
| CN106099069A (en) * | 2016-08-15 | 2016-11-09 | 华南理工大学 | A kind of sodium-ion battery negative pole SnS/C composite and preparation method thereof |
| CN109360953A (en) * | 2018-09-28 | 2019-02-19 | 天津大学 | A kind of method synthesizing vulcanization lithium/carbon composite material and the lithium-sulfur cell using the material |
| CN110137462A (en) * | 2019-05-10 | 2019-08-16 | 浙江大学 | Preparation method for aluminium/lithium sulphide battery vulcanization lithium/carbon composite material |
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