CN113582155A - Biomass charcoal intermediate layer and preparation method and application thereof - Google Patents
Biomass charcoal intermediate layer and preparation method and application thereof Download PDFInfo
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- CN113582155A CN113582155A CN202110727885.5A CN202110727885A CN113582155A CN 113582155 A CN113582155 A CN 113582155A CN 202110727885 A CN202110727885 A CN 202110727885A CN 113582155 A CN113582155 A CN 113582155A
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Abstract
The invention provides a biomass charcoal intermediate layer and a preparation method and application thereof, which comprises the steps of pretreating a fibrous biomass material to obtain a first precursor; calcining and cooling the first precursor under a protective atmosphere to obtain biomass charcoal; and tabletting and cutting the biomass charcoal to obtain the biomass charcoal intermediate layer. The intermediate layer prepared by the invention has a one-dimensional hollow tube structure, can provide a large number of lithium ion transmission channels and abundant pore structures, so that polysulfide can be more effectively adsorbed, and the cycle stability of the lithium-sulfur battery is greatly improved. Meanwhile, the biomass charcoal has the advantages of wide source, low manufacturing cost and the like, can greatly save the production cost, and is beneficial to industrial production.
Description
Technical Field
The invention belongs to the technical field of lithium-sulfur batteries, and particularly belongs to a biomass charcoal interlayer and a preparation method and application thereof.
Background
At the end of the twentieth century, lithium ion batteries successfully achieve commercial application and then have been widely researched and applied, but now with the bottleneck of development of pure lithium ion batteries, lithium sulfur batteries with the advantages of high energy density, low cost, environmental friendliness and the like have attracted extensive attention and research.
However, the disadvantages of the lithium-sulfur battery greatly hinder the commercial application of the lithium-sulfur battery, wherein the "shuttle effect" is one of the main factors influencing the performance of the lithium-sulfur battery, positive electrode sulfur is converted into polysulfide which is soluble in organic electrolyte during the discharge process and penetrates through a diaphragm to reach a negative electrode area to form the "shuttle effect", so that the utilization rate of active materials in the lithium-sulfur battery is reduced, and the electrochemical performance of the lithium-sulfur battery is further influenced, and the research on the intermediate layer is one of the important ways for solving the "shuttle effect".
The added intermediate layer between the diaphragm and the positive electrode can be used as a second current collector to improve the conductivity of the positive electrode of the lithium sulfur battery on one hand, and can inhibit the occurrence of a shuttle effect by adsorbing polysulfide on the other hand, thereby improving the electrochemical performance of the lithium sulfur battery. Therefore, research into an intermediate layer of a lithium-sulfur battery having superior performance is an important method for improving the performance of the lithium-sulfur battery.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the biomass charcoal intermediate layer and the preparation method and the application thereof, the biomass charcoal has the advantages of wide source, low manufacturing cost and the like, the production cost can be greatly saved, the industrial production is facilitated, and the cycling stability of the lithium-sulfur battery can be greatly improved by using the biomass charcoal intermediate layer.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a biomass charcoal intermediate layer comprises the following specific steps:
s1, pretreating the fibrous biomass material to obtain a first precursor;
s2, calcining and cooling the first precursor under a protective atmosphere to obtain biomass charcoal;
s3, tabletting and cutting the biomass charcoal to obtain the biomass charcoal intermediate layer.
Further, in step S1, the fibrous biomass material is waste cotton soft tissue or waste cotton fiber fabric.
Further, in step S1, the pretreatment is to acid wash the fibrous biomass material.
Further, the acid washing is to soak the fiber biomass material in hydrochloric acid with the concentration of 0.2mol/L-1.5mol/L for 2h-5h, wash the fiber biomass material with water after the acid washing to be neutral, and dry the fiber biomass material to obtain a first precursor.
Further, in step S2, the protective atmosphere is nitrogen, argon, or a mixture thereof.
Further, in step S2, the calcining is carried out in a tubular furnace at a high temperature of 600-900 ℃ for 2-5 h, and the biomass charcoal is obtained after cooling to room temperature.
Further, in step S3, a cutting machine is used for the cutting.
Further, in step S3, the thickness of the biomass charcoal intermediate layer is 0.09mm to 0.11 mm.
The invention also provides a biomass charcoal intermediate layer which is prepared by the preparation method and is provided with a one-dimensional hollow tube structure.
The invention also provides an application of the biomass charcoal intermediate layer in preparation of a lithium-sulfur battery, wherein the lithium-sulfur battery has 536mAh & g under the charge-discharge current density of 0.5C-1The initial specific capacity of the alloy is 449mAh g after 100 times of circulation-1Average capacity fade of 0.16% per cycle.
Compared with the prior art, the invention has at least the following beneficial effects:
according to the preparation method of the biomass charcoal intermediate layer, the fibrous biomass material is pretreated and then subjected to a one-step carbonization method to obtain the biomass charcoal intermediate layer, the biomass charcoal intermediate layer can be used as an upper layer current collector to greatly improve the specific capacity and rate performance of the lithium sulfur battery, a migration path of polysulfide can be increased by using a porous adsorption method through a physical adsorption method, and polysulfide can be adsorbed by using a chemical bond formed between an intermediate layer material and the polysulfide through a chemical adsorption method, so that the effect of improving the performance of the lithium sulfur battery is achieved; the preparation method disclosed by the invention is simple to operate, can greatly reduce time and economic cost, is more favorable for commercial production, and is expected to be applied to the fields of energy storage systems and new energy.
The biomass charcoal obtained in the invention has a one-dimensional hollow tube structure, so that channels for lithium ion transportation in the intermediate layer can be increased, and the electrochemical performance of the lithium-sulfur battery is improved. On the other hand, the specific surface area of the intermediate layer can be increased so as to more effectively convert and adsorb polysulfide, thereby inhibiting the shuttle effect and improving the cycle stability of the lithium-sulfur battery and the utilization rate of polysulfide.
The waste cotton soft towel or the waste cotton fiber fabric is used as the biomass carbon-based material, so that the conductivity and the adsorption performance are good, the middle layer made of the waste cotton soft towel or the waste cotton fiber fabric has a certain adsorption effect on polysulfide generated by oxidation-reduction reaction in the lithium-sulfur battery, and the cycle performance of the battery is further effectively improved.
Drawings
Fig. 1 is an SEM image of biomass char prepared in step two of example 1 of the present invention.
FIG. 2 is a diagram showing the pore size distribution of biomass char prepared in step two of example 1 of this experiment.
Fig. 3 is an adsorption curve diagram of biomass charcoal prepared in step two of experimental example 1.
Fig. 4 is a cycle graph of a lithium sulfur battery using a biomass charcoal interlayer prepared in example 1 of the present invention.
Fig. 5 is a charge and discharge graph of a lithium sulfur battery using a biomass charcoal interlayer prepared in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and detailed description, which will be given in detail below with reference to specific examples, which are intended to illustrate and not to limit the present invention.
The invention provides a preparation method of a biomass charcoal intermediate layer, which comprises the following steps:
(1) the fiber biomass material is soaked in 0.2-1.5 mol/L hydrochloric acid for 2-5 h for acid washing, then washed to be neutral, and dried to obtain a first precursor.
(2) And (3) placing the first precursor into a tubular furnace filled with nitrogen, argon or a mixed gas of the nitrogen and the argon, calcining at the high temperature of 600-900 ℃ for 2-5 h, and cooling to room temperature to obtain the biomass charcoal.
(3) And tabletting the biomass carbon to obtain a biomass carbon layer with the thickness of 0.09mm-0.11mm, and cutting by using a cutting machine to obtain the biomass carbon intermediate layer.
Preferably, the fiber biomass material is waste cotton soft towel or waste cotton fiber fabric;
preferably, the biomass charcoal layer is cut into a circular shape with the diameter of 16mm, and can be used as a button cell intermediate layer, or can be cut into an intermediate layer with the diameter of 2mm-50mm according to other types of batteries.
Example 1:
the method comprises the following steps: and soaking the waste cotton soft towel in 0.2mol/L hydrochloric acid for 5h for acid washing, then washing with water to be neutral, and drying to obtain a first precursor.
Step two: and (3) placing the first precursor in the first step into a tube furnace filled with nitrogen, heating for 3h at 800 ℃, and cooling to room temperature to obtain the biomass charcoal.
Step three: and (4) tabletting the biomass charcoal prepared in the step two to obtain a biomass charcoal layer with the thickness of 0.09mm, and cutting the biomass charcoal layer into a circular middle layer with the diameter of 16mm by using a cutting machine to finish the preparation of the middle layer.
Fig. 1 is an SEM image of the biomass charcoal intermediate layer prepared in example 1, and it can be seen from the SEM image that the prepared intermediate layer has a one-dimensional hollow tube structure, and can play a role in physically blocking and inhibiting diffusion of polysulfides, thereby improving the utilization rate of active materials and the specific capacity of the battery.
Fig. 2 is a pore size distribution diagram of the biomass charcoal in example 1, and fig. 3 is an adsorption curve diagram of the biomass charcoal in example 1, the specific surface area of the material is 519.92m2/g, and the total pore volume is 0.15cm3/g, which shows that the material has a rich pore structure, mainly comprising micropores and mesopores, so that the biomass charcoal material can greatly inhibit the "shuttle effect", thereby improving the electrochemical performance of the lithium-sulfur battery.
Fig. 4 is a graph showing the cycle profile of a lithium sulfur battery prepared using the biomass charcoal interlayer prepared in example 1, from which it can be seen that the presence of the interlayer significantly improves the electrochemical performance.
Fig. 5 is a charge-discharge curve diagram of a lithium sulfur battery prepared by using the biomass charcoal interlayer prepared in example 1, and the polarization phenomenon of the lithium sulfur battery can be greatly reduced and the electrochemical performance of the lithium sulfur battery can be effectively improved by using the interlayer.
Example 2:
the method comprises the following steps: and soaking the waste cotton soft towel in 0.4mol/L hydrochloric acid for 5h for acid washing, then washing with water to be neutral, and drying to obtain a first precursor.
Step two: and (3) placing the first precursor in the first step into a tubular furnace filled with argon, heating for 2h at 900 ℃, and cooling to room temperature to obtain the biomass charcoal.
Step three: and D, tabletting the biomass charcoal prepared in the step two to obtain a biomass charcoal layer with the thickness of 0.11mm, and cutting the biomass charcoal layer into a circular middle layer with the diameter of 2mm by using a cutting machine, thus finishing the preparation of the middle layer.
Example 3:
the method comprises the following steps: and (3) soaking the waste pure cotton fabric clothes for 4h by using 0.6mol/L hydrochloric acid for pickling, then washing the clothes to be neutral, and drying the clothes to obtain a first precursor.
Step two: and (3) placing the first precursor in the first step into a tubular furnace into which mixed gas of nitrogen and argon is introduced, heating for 4 hours at 700 ℃, and cooling to room temperature to obtain the biomass charcoal.
Step three: and D, tabletting the biomass charcoal prepared in the step two to obtain a biomass charcoal layer with the thickness of 0.10mm, and cutting the biomass charcoal layer into a circular middle layer with the diameter of 50mm by using a cutting machine, thus finishing the preparation of the middle layer.
Example 4:
the method comprises the following steps: and (3) soaking the waste long stapled cotton fiber fabric for 3 hours by using 0.8mol/L hydrochloric acid for pickling, then washing the fabric to be neutral, and drying the fabric to obtain a first precursor.
Step two: and (3) placing the first precursor in the first step into a tube furnace filled with nitrogen, heating for 5h at 600 ℃, and cooling to room temperature to obtain the biomass charcoal.
Step three: and D, tabletting the biomass charcoal prepared in the step two to obtain a biomass charcoal layer with the thickness of 0.11mm, and cutting the biomass charcoal layer into a circular middle layer with the diameter of 16mm by using a cutting machine, thus finishing the preparation of the middle layer.
Example 5:
the method comprises the following steps: and soaking the waste short staple cotton fiber fabric in 1.5mol/L hydrochloric acid for 2h for acid washing, then washing with water to be neutral, and drying to obtain a first precursor.
Step two: and (3) placing the first precursor in the first step in a tubular furnace filled with nitrogen, heating for 5 hours at 750 ℃, and cooling to room temperature to obtain the biomass charcoal.
Step three: and D, tabletting the biomass charcoal prepared in the step two to obtain a biomass charcoal layer with the thickness of 0.09mm, and cutting the biomass charcoal layer into a circular middle layer with the diameter of 16mm by using a cutting machine, thus finishing the preparation of the middle layer.
The lithium-sulfur battery using the intermediate layer has 536mAh g at a charge-discharge current density of 0.5C-1The initial specific capacity of (a). After 100 times of circulation, the specific capacity can still reach 449mAh g-1The average capacity of the battery per cycle is only attenuated by 0.16%, and the battery has good cycle performance. While the lithium-sulfur battery without the intermediate layer had 505mAh g at a charge-discharge current density of 0.5C-1The initial specific capacity of (a). After 100 times of circulation, the specific capacity only remains 200mAh g-1The cycle performance of the battery is poor.
Claims (10)
1. A preparation method of a biomass charcoal intermediate layer is characterized by comprising the following specific steps:
s1, pretreating the fibrous biomass material to obtain a first precursor;
s2, calcining and cooling the first precursor under a protective atmosphere to obtain biomass charcoal;
s3, tabletting and cutting the biomass charcoal to obtain the biomass charcoal intermediate layer.
2. The method for preparing the biomass charcoal interlayer according to claim 1, wherein in step S1, the fibrous biomass material is waste cotton soft tissue or waste cotton fiber fabric.
3. The method for preparing the biomass charcoal intermediate layer according to claim 1, wherein the pretreatment is acid washing of the fibrous biomass material in step S1.
4. The method for preparing the biomass charcoal intermediate layer according to claim 3, wherein the acid washing is to soak the fibrous biomass material in hydrochloric acid with a concentration of 0.2mol/L to 1.5mol/L for 2h to 5h, wash the fibrous biomass material with water to be neutral after the acid washing, and dry the fibrous biomass material to obtain the first precursor.
5. The method of claim 1, wherein in step S2, the protective atmosphere is nitrogen, argon, or a mixture thereof.
6. The method for preparing the biomass charcoal interlayer as claimed in claim 1, wherein in step S2, the calcination is performed at a high temperature of 600-900 ℃ in a tube furnace for 2-5 h, and the biomass charcoal is obtained after cooling to room temperature.
7. The method for preparing the biomass charcoal intermediate layer according to claim 1, wherein in step S3, a cutting machine is used for cutting.
8. The method for preparing the biomass charcoal intermediate layer according to claim 1, wherein in step S3, the thickness of the biomass charcoal intermediate layer is 0.09mm to 0.11 mm.
9. A biomass charcoal intermediate layer produced by the production method according to any one of claims 1 to 9, the biomass charcoal intermediate layer having a one-dimensional hollow tube structure.
10. The use of a biochar interlayer as in claim 9, wherein the biochar interlayer is used to make a lithium sulfur cell having 536 mAh-g at a charge-discharge current density of 0.5C-1The initial specific capacity of the alloy is 449mAh g after 100 times of circulation-1Average capacity fade of 0.16% per cycle.
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Citations (4)
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| US20090068545A1 (en) * | 2007-09-11 | 2009-03-12 | Korea Institute Of Energy Research | Method of manufacturing cellulose electrode for fuel cells, cellulose electrode manufactured thereby, and use of cellulose fibers as fuel cell electrodes |
| WO2020010750A1 (en) * | 2018-07-09 | 2020-01-16 | 华南理工大学 | Nitrogen-doped 3d porous carbon material, preparation method therefor and use thereof |
| US20200112019A1 (en) * | 2017-12-08 | 2020-04-09 | Lg Chem, Ltd. | Negative electrode active material for lithium secondary battery and method for preparing the same |
| CN111847418A (en) * | 2019-04-24 | 2020-10-30 | 香港理工大学深圳研究院 | Preparation method and application of biomass hard carbon for negative electrode material of sodium-ion battery |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090068545A1 (en) * | 2007-09-11 | 2009-03-12 | Korea Institute Of Energy Research | Method of manufacturing cellulose electrode for fuel cells, cellulose electrode manufactured thereby, and use of cellulose fibers as fuel cell electrodes |
| US20200112019A1 (en) * | 2017-12-08 | 2020-04-09 | Lg Chem, Ltd. | Negative electrode active material for lithium secondary battery and method for preparing the same |
| WO2020010750A1 (en) * | 2018-07-09 | 2020-01-16 | 华南理工大学 | Nitrogen-doped 3d porous carbon material, preparation method therefor and use thereof |
| CN111847418A (en) * | 2019-04-24 | 2020-10-30 | 香港理工大学深圳研究院 | Preparation method and application of biomass hard carbon for negative electrode material of sodium-ion battery |
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| ZHENG BANGBEI. ET AL: "Waste cotton cloth derived carbon microtube textile: a robust and scalable interlayer for lithium–sulfur batteries", CHEMICAL COMMUNICATIONS * |
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