CN109755469B - Lamellar electrode for lithium-sulfur battery and preparation and application thereof - Google Patents
Lamellar electrode for lithium-sulfur battery and preparation and application thereof Download PDFInfo
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Abstract
The invention relates to a lamellar porous electrode for a lithium-sulfur battery and preparation and application thereof.A low-freezing-point solvent is selected to prepare active substance slurry, and a lamellar electrode is prepared by a freeze-drying method; the preparation method of the lamellar electrode is simple, the process is environment-friendly, the material structure is stable, and the lamellar electrode structure is beneficial to improving the performance of the Li-S battery with high load.
Description
Technical Field
The invention relates to an electrode material for a lithium-sulfur battery.
Background
In the past 20 years, lithium ion batteries have been rapidly developed and rapidly occupy the battery field of portable electronic products such as mobile phone batteries and mobile power supplies. However, the theoretical specific capacity of the lithium ion battery based on the 'de-intercalation' theory is less than 300mA h g-1Actual energy density of less than 200Wh kg-1And the requirements of people on electronic equipment, electric automobiles and unmanned planes cannot be met. As a new electrochemical energy storage secondary battery, the lithium-sulfur battery is different from the traditional rocking chair type lithium ion battery, and in the discharging process, the active substance sulfur and the metal lithium generate two-electron reaction, so that 1675mAh g is released-1Theoretical specific capacity of 2600Wh kg-1The energy ratio of the sulfur-containing active substance is high, and the sulfur-containing active substance has the advantages of high natural abundance, low cost, low toxicity, environmental friendliness and the like. Therefore, the lithium-sulfur battery is considered to be one of novel secondary batteries capable of replacing lithium ion batteries, and has good application prospects.
However, the materials and systems of lithium sulfur batteries still face many challenges: 1) elemental sulfur as active material and lithium sulfide Li as discharge product2S poor conductivity (conductivity about 10)-30S cm-1) Further leading to poor electrochemical contact inside the sulfur positive electrode, thereby causing larger internal impedance of the battery; 2) the difference in density between sulfur and lithium sulfide causes nearly 80% volume expansion during discharge; 3) the polysulfide of the reaction intermediate product shuttles between a positive pole and a negative pole under the influence of electric field force and concentration gradient in the charging process,and can generate side reaction with a sulfur anode and a lithium cathode, and the coulomb efficiency is reduced; 4) the ether electrolyte reacts with the metal lithium to form lithium dendrite on the surface of the negative electrode, thereby causing safety problems; 5) the surface of the metal lithium is passivated to form an SEI film, so that the effective reaction sites of the metal lithium are reduced, and further reaction is hindered. Therefore, poor cycle performance and low rate performance restrict the industrial development of the Li-S battery. Starting from the positive electrode material of the lithium-sulfur battery, the main problems can be effectively solved.
Li-S batteries have rapidly developed in recent years with sulfur loadings of less than 2mg cm-2In the process, the cycle performance and the rate performance of the composite material are greatly improved. Although the low-supported electrode can effectively alleviate many problems, its lower energy density cannot satisfy the practical requirements! Therefore, high-supported lithium-sulfur batteries are being developed to achieve higher energy densities. However, the electrochemical performance of the high-load battery is poor, and the main reason is that 1, when the high-load electrode is prepared based on a blade coating method, the electrode is easy to crack, and the active substance is easy to fall off, so that the electrode is unstable when reacting in the battery; 2 the internal mass transfer of the high-load electrode is poor, the electronic conduction and ion transmission in the electrode are limited, and sufficient electrons and ions cannot be provided for the reaction. The invention provides the lamellar porous electrode, so that the mass transfer in the electrode is improved, a faster electron and ion transmission path is provided for electrode reaction, the reaction is accelerated, and the cycle performance and the rate performance of the battery are improved.
Disclosure of Invention
In order to solve the above technical problems, the present invention aims to provide a lamellar electrode and its application in a lithium-sulfur battery.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a positive electrode material for a lithium-sulfur battery,
selecting a low-freezing-point solvent, using soluble high-molecular resin as a binder, mixing a carbon/sulfur compound and conductive carbon, coating the mixture on a substrate, and preparing a lamellar electrode on the substrate by a freeze-drying method;
the low freezing point solvent is water or camphene; preferably: water;
when the solvent is water, the binder is one or more of LA series, carboxymethyl cellulose-styrene butadiene rubber (CMC-SBR), beta-cyclodextrin, polyvinyl alcohol and the like; preferably: when the solvent is camphene, CMC-SBR does not need high molecular resin as a binder, but needs a mould as a template;
the carbon/sulfur compound is one or more than two compounds of carbon materials and sulfur. The carbon material is one or more than two of carbon nano tube, graphene, carbon nano fiber, BP2000, KB600, KB300, XC-72, Super-P, acetylene black, activated carbon or carbon materials modified or activated by the carbon nano tube, the graphene, the carbon nano fiber, the BP2000, the KB600, the KB300, the XC-72, the Super-P, the acetylene black and the activated carbon.
The conductive carbon may be one or more of the above carbon materials, and is preferably graphene.
The lamellar electrode can be designed into a micropore, mesopore or macropore structure.
The thickness of the lamellar electrode is 20-500 mu m, the pore size is 0.5-5000 nm, the porosity is 10-90%, and the porosity is preferably 70%.
The weight of the soluble polymer resin of the lamellar electrode accounts for 2-40 wt% of the total weight of the electrode.
The mass of sulfur in the thin-layer electrode and the carbon-sulfur composite accounts for 20-80 wt% of the total mass.
The preparation method of the electrode comprises the following steps:
when the low freezing point solvent is selected as water:
(1) adding a binder into water, and stirring for 0.5-2 hours at the temperature of 20-50 ℃ to form a high polymer solution with the mass concentration of 2-40%; adding a carbon/sulfur compound or a mixture of the carbon/sulfur compound and a carbon material into the solution, and fully stirring for 2-10 hours at the temperature of 20-50 ℃ to prepare slurry; wherein the solid content is between 5 and 40 weight percent, preferably 20 to 30 weight percent;
(2) pouring the slurry prepared in the step (1) on a substrate, carrying out blade coating, and then placing the substrate in a low-temperature environment A (-200 ℃ to-10 ℃) until the solvent is completely solidified; wherein the scraping amount controls the loading amount of sulfur to be 0.5-20mg/cm2(ii) a The loading amount is preferably 4-8mg/cm2(ii) a The substrate is one of aluminum foil, copper foil, carbon paper or carbon felt；
(3) Vacuum drying the solidified body obtained in the step 2) for 6-24 hours in a low-temperature environment B (-200 ℃ to-10 ℃) to prepare a lamellar electrode;
(4) drying the thin-layer electrode prepared in the step (3) at room temperature to 100 ℃ for 2-24 h to obtain a dried thin-layer electrode;
when the low freezing point solvent is selected as camphene:
(1) directly adding carbon/sulfur compound or carbon/sulfur compound and conductive carbon into camphene, and fully stirring for 2-10 h at the temperature of 50-100 ℃ to prepare slurry; wherein the solid content is between 5 and 40 weight percent, preferably 20 to 30 weight percent;
(2) pouring the slurry prepared in the step (1) into a specific mould, and then placing the mould in a low-temperature environment C (-200-40 ℃) until the solvent is completely solidified; wherein the amount of the poured slurry is controlled to control the loading amount of sulfur to be 0.5-20mg/cm2(ii) a The loading amount is preferably 2-5mg/cm2；
(3) Vacuum drying the solidified body obtained in the step (2) for 6-24h in a low-temperature environment D (-200 ℃ -40 ℃) to prepare a lamellar electrode;
(4) drying the thin-layer electrode prepared in the step (3) at room temperature to 100 ℃ for 2-24 h to obtain a dried thin-layer electrode;
carbon/sulfur composite in mixture of carbon/sulfur composite and conductive carbon: the ratio of conductive carbon is 2-19;
the lamellar electrode is used as a positive electrode in a lithium-sulfur battery.
The beneficial results of the invention are:
(1) when the electrode is prepared, the non-toxic aqueous gel is used for replacing the traditional polyvinylidene fluoride (PVDF), so that the toxic solvent N-dimethyl pyrrolidone (NMP) is prevented from harming human bodies and the environment;
(2) the freeze drying method is adopted to replace the traditional oven drying method, so that the problems of electrode cracking, active substance falling and the like in the traditional method are solved, and the method can be used for preparing high-load electrodes;
(3) the electrode prepared by the method is of a lamellar porous structure, has high porosity, is beneficial to adsorbing more electrolyte, and can fix polysulfide dissolved in the electrolyte on one side of the positive electrode under the synergistic action of the electrode and the lamellar electrode, so that the flying shuttle of the polysulfide is reduced, and the cycle performance of the battery is improved;
(4) the electrode prepared by the invention is of a vertical porous thin-layer structure, the longitudinal thick electrode of a high-load battery is converted into the transverse thin electrode, the transmission path of lithium ions is shortened, and meanwhile, the layered structure also provides a continuous conduction network for the conduction of electrons, so that the mass transfer process in the battery is accelerated, and the rate capability of the battery is improved;
the porous electrode with the vertically distributed thin layers prepared by the invention has good ion transmission capability, polysulfide is effectively fixed by the special layered electrode structure, and the lithium ion transmission path is shortened by the thin layered structure, so that the rate capability and the cycle performance of the battery are excellent, and the preparation process is simple and environment-friendly. The porous lamellar electrode which is vertically distributed is used as the anode material of the lithium-sulfur battery, so that the cycle performance and the rate capability of the battery are effectively improved.
Drawings
FIG. 1: photographs of comparative example electrodes (upper panel) and example electrodes (lower panel) with different sulfur loading;
FIG. 2: SEM images of the preferred example surface (a, b), comparative example surface (c, d), and example surface (e, f);
FIG. 3: a comparative example sectional SEM image (a), an example sectional SEM image (b) and a preferred example sectional SEM image (c);
FIG. 4: the porosity of the comparative example, the example and the preferred example is compared;
FIG. 5: comparing the liquid absorption rates of the comparative example and the example with those of the preferred example;
FIG. 6: rate performance test of lithium-sulfur batteries assembled by using comparative examples, examples and preferred examples;
FIG. 7: testing the cycle stability of the lithium-sulfur battery assembled by using the comparative example, the example and the preferred example;
FIG. 8: cycling stability testing of high supported lithium sulfur batteries assembled in the preferred examples.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to limit the scope of the present invention.
Carbon-sulfur composite preparation was carried out by placing 10g of commercial KB600 in a tube furnace under Ar protection at 5 ℃ for min-1Heating to 900 deg.C, introducing steam for activation for 1.5h, wherein the flow rate of steam is 600mL min-1The activated carbon material was designated A-KB 600. Mixing 5g A-KB600 and 10g S, heating to 155 deg.C in a tube furnace at a heating rate of 1 deg.C for min-1And keeping the temperature for 20h to obtain the product which is marked as S/A-KB 600.
Comparative example
Dissolving 0.03g of carboxymethyl cellulose (CMC) in 3g of deionized water, stirring for 1h, adding 0.8g S/A-KB600 and 0.1g of KB600, stirring for 5h, adding 0.15g of 40 wt% styrene-butadiene rubber (SBR), stirring at a slow speed for 0.5h, adjusting a scraper to 300 mu m, blade-coating on an aluminum film to form a film, drying at 70 ℃ overnight, shearing into small round pieces with the diameter of 14mm, weighing, vacuum drying at 60 ℃ for 24h, and taking the small round pieces coated with S/KB600 as a positive electrode (the sulfur loading of each round piece is about 1.5mg cm)-2) Lithium sheet as negative electrode, celgard 2325 as diaphragm, 1M lithium bis (trifluoromethylsulfonyl) imide solution (LiTFSI) plus 1% LiNO3The electrolyte solution was a mixed solution of 1, 3-Dioxolane (DOL) and ethylene glycol dimethyl ether (DME) (volume ratio v/v 1:1), the cells were assembled, and the cell cycle performance test was performed at 0.2C rate and the rate performance test was performed at 0.1C to 2C rate.
The first-turn specific discharge capacity under 0.2C multiplying power is 907mA h g-1The specific capacity is maintained at 610mA h g after 100 cycles-1The capacity retention rate is 67.3%; when the multiplying power is increased to 2C, the specific discharge capacity is 451mA h g-1。
Example 1
Dissolving 0.03g of carboxymethyl cellulose (CMC) in 3g of deionized water, stirring for 1h, adding 0.8g S/A-KB600 and 0.1g of KB600, stirring for 5h, adding 0.15g of 40 wt% Styrene Butadiene Rubber (SBR), stirring at a slow speed for 0.5h, adjusting a scraper to 300 mu m, blade-coating on an aluminum film to form a film, quickly immersing the film in liquid nitrogen, taking out after 10min, quickly transferring to a freeze dryer (the temperature is-50 ℃, the vacuum degree is less than 10), drying for 10h, and drying at 50 ℃ overnight. Subsequent electrode preparation and cell assembly were the same as in the comparative example.
The first-circle specific discharge capacity under 0.2C multiplying power is 926mA h g-1The specific capacity is maintained to be 721mA h g after 100 cycles-1The capacity retention rate is 77.9%; when the multiplying power is increased to 2C, the specific discharge capacity is mA h g-1。
EXAMPLE 2 (preferred example)
Dissolving 0.03g of carboxymethyl cellulose (CMC) in 4g of deionized water, stirring for 1h, adding 0.8g S/A-KB600 and 0.1g of graphene, stirring for 5h, adding 0.15g of 40 wt% Styrene Butadiene Rubber (SBR), stirring slowly for 0.5h, adjusting a scraper to 300 mu m and 1000 mu m (the sulfur loading per chip is about 8mg cm)-2) Spreading on aluminum film to form film, rapidly immersing in liquid nitrogen for 10min, taking out, and rapidly transferring to freeze drier (temperature-50 deg.C, vacuum degree)<10) Drying for 10h, and drying at 50 ℃ overnight. Subsequent electrode preparation and cell assembly were the same as in the comparative example.
The first-circle discharge specific capacity under 0.2C multiplying power is 1203mA h g-1The specific capacity is maintained to be 768mA h g after 100 cycles-1The capacity retention was 78.3% (calculated based on the third round); when the multiplying power is increased to 2C, the specific discharge capacity is 675mA h g-1。
As can be seen from FIG. 1, the supporting amount of the comparative electrode is 1.5mg cm-2In this case, the electrode was cracked, and the active material gradually fell off from the Al foil with an increase in the supporting amount. The electrode of the embodiment is flat, no obvious defect is seen, close connection is kept between the electrode and the current collector, and the supporting quantity can be increased to 15mg cm-2. Preferred examples are prepared in the same manner as examples, using different conductive carbons and at different solids contents, and thus the macro-topography is similar to the examples. However, from the microscopic topography shown in fig. 2, the example and preferred electrodes are porous laminar electrodes, with a large number of pore channels evident in cross-section (shown in fig. 3), and the electrodes are in close contact with the current collector. The electrode of the preferred embodiment has more proper solid content, so the layered structure is more uniform and the channels are more obvious. Whereas conventional oven-dried electrodes are island-shaped (as shown in fig. 2b, d), the connection to the current collector is not tight enough. As shown in FIGS. 4 and 5, the liquid absorption rates of the electrodes of the examples and preferred examplesThe porosity is high, which is beneficial to the ion transmission in the electrode. Based on the above characteristics of the porous lamellar electrode, as shown in fig. 6, the battery using the embodiments and preferred examples as the positive electrode material has better rate performance, which is probably because 1) the contact between the material in the lamellar electrode and the substrate is better, which is beneficial to the transfer of electrons; 2) the electrode is not cracked and has a layered structure, and a continuous electronic conduction network is provided for electronic conduction; 3) the thin-layer porous electrode has high porosity and provides sufficient Li for the micro-reaction region+(ii) a 4) The porous layered electrode shortens an ion transmission path and accelerates ion transmission. Compared with the comparative example, the battery using the examples and the preferred examples as the positive electrode material has better cycle stability (as shown in fig. 7), on one hand, the electrode surface is flat, no crack occurs, meanwhile, the layered structure of the electrode is beneficial to blocking the shuttle of polysulfide, and on the other hand, the liquid absorption rate of the porous layered electrode is higher, which means that more electrolyte with polysulfide dissolved is fixed on one side of the positive electrode, the shuttle effect is relieved, and the cycle stability of the battery is improved. The preferred embodiment has more proper solid content, uniform layered structure and more moderate pore structure, and is beneficial to the rapid transmission of ions because better electrochemical performance is obtained.
In addition, the preferred embodiment can also prepare a high-supported electrode (8mg cm)-2) The discharge specific capacity of the battery assembled by the lithium ion battery is stabilized at 769mAh g at 0.1C-1And the capacity retention rate after 75 cycles is 87.6%, and the specific electrochemical performance is shown in FIG. 8. The application prospect of the porous layered electrode in the high-load lithium-sulfur battery is demonstrated.
Claims (10)
1. A laminar electrode for a lithium sulfur battery characterized in that:
selecting a low-freezing-point solvent, blending the carbon/sulfur compound and the carbon material mixture in the low-freezing-point solvent, and preparing the lamellar electrode by a freeze-drying method; the low freezing point solvent is water or camphene; the electrodes are of a thin-layer structure, the thin-layer structure is perpendicular to the substrate and distributed, the distance between thin layers is 0.05-10 mu m, and the thickness of the thin layers is 0.05-10 mu m; the thin layer is of a porous structure, and the pores comprise micropores, mesopores and macropores, wherein the micropores are less than 2 nm, the mesopores are 2-50 nm, and the macropores are 50-5000 nm, and the micropore volume accounts for 20-70% of the total pore volume; carbon/sulfur complex in mixture of carbon/sulfur complex and carbon material: the proportion of the carbon material is 2-19; the carbon material is graphene;
the thin-layer electrode prepared by the freeze-drying method is prepared by the following specific processes,
when the low freezing point solvent is selected as water:
(1) adding a binder into water, and stirring for 0.5-2 hours at the temperature of 20-50 ℃ to form a high polymer solution with the mass concentration of 2-40%; adding a mixture of a carbon/sulfur compound and a carbon material into the solution, and fully stirring for 2-10 hours at the temperature of 20-50 ℃ to prepare slurry; wherein the solid content is 5-40 wt%;
(2) pouring the slurry prepared in the step (1) on a substrate, carrying out blade coating to form a film, quickly immersing the film in liquid nitrogen, taking out the film after 10min, and completely solidifying the solvent; wherein the scraping amount controls the loading amount of sulfur to be 0.5-20mg/cm2(ii) a The substrate is one of aluminum foil, copper foil, carbon paper or carbon felt;
(3) vacuum drying the solidified body obtained in the step 2) for 6-24 hours in a low-temperature environment B to prepare a lamellar electrode;
(4) drying the thin-layer electrode prepared in the step (3) at room temperature to 100 ℃ for 2-24 hours to obtain a dried thin-layer electrode;
wherein the low-temperature environment B ranges from minus 200 ℃ to minus 10 ℃;
when the low freezing point solvent is selected as camphene:
(1) directly adding the carbon/sulfur compound and the carbon material into camphene, and fully stirring for 2-10 h at the temperature of 50-100 ℃ to prepare slurry; wherein the solid content is 5-40 wt%;
(2) pouring the slurry prepared in the step (1) into a mold, quickly immersing the mold into liquid nitrogen, taking out the mold after 10min until the solvent is completely solidified; wherein the amount of the poured slurry is controlled to control the loading amount of sulfur to be 0.5-20mg/cm2；
(3) Vacuum drying the solidified body obtained in the step (2) for 6-24 hours in a low-temperature environment D to prepare a lamellar electrode;
(4) drying the thin-layer electrode prepared in the step (3) at room temperature to 100 ℃ for 2-24 hours to obtain a dried thin-layer electrode;
wherein the low-temperature environment D ranges from-200 ℃ to 40 ℃.
2. The electrode of claim 1, wherein:
when the low freezing point solvent is selected as water: in the step (1), the solid content is 20-30 wt%; the supporting capacity in the step (2) is 4-8mg/cm2；
When the low freezing point solvent is selected as camphene: in the step (1), the solid content is 20-30 wt%; in the step (2), the supporting capacity is 2-5mg/cm2。
3. The electrode of claim 1, wherein: when the low freezing point solvent is water, the binder is one or more than two of LA series, carboxymethyl cellulose-styrene butadiene rubber (CMC-SBR), beta-cyclodextrin and polyvinyl alcohol.
4. The electrode of claim 3, wherein: when the low freezing point solvent is water, the binder is CMC-SBR.
5. The electrode of claim 1, wherein: the carbon/sulfur compound is a compound of a carbon material and sulfur, wherein the mass of the sulfur accounts for 20-80 wt% of the total mass of the carbon/sulfur compound.
6. The electrode of claim 1, wherein: the thickness of the electrode is 20-900 μm, and the porosity is 10-90%.
7. The electrode of claim 6, wherein: the electrode porosity was 70%.
8. A method for preparing a laminar electrode according to any of claims 1 to 7, characterized in that: carbon/sulfur complex in mixture of carbon/sulfur complex and carbon material: the proportion of the carbon material is 2-19, and the carbon material is graphene;
the thin-layer electrode is prepared by the following process,
when the low freezing point solvent is selected as water:
(1) adding a binder into water, and stirring for 0.5-2 hours at the temperature of 20-50 ℃ to form a high polymer solution with the mass concentration of 2-40%; adding a mixture of a carbon/sulfur compound and a carbon material into the solution, and fully stirring for 2-10 hours at the temperature of 20-50 ℃ to prepare slurry; wherein the solid content is 5-40 wt%;
(2) pouring the slurry prepared in the step (1) on a substrate, carrying out blade coating to form a film, quickly immersing the film in liquid nitrogen, taking out the film after 10min, and completely solidifying the solvent; wherein the scraping amount controls the loading amount of sulfur to be 0.5-20mg/cm2(ii) a The substrate is one of aluminum foil, copper foil, carbon paper or carbon felt;
(3) vacuum drying the solidified body obtained in the step 2) for 6-24 hours in a low-temperature environment B to prepare a lamellar electrode;
(4) drying the thin-layer electrode prepared in the step (3) at room temperature to 100 ℃ for 2-24 hours to obtain a dried thin-layer electrode;
the low-temperature environment B ranges from minus 200 ℃ to minus 10 ℃;
when the low freezing point solvent is selected as camphene:
(1) directly adding the carbon/sulfur compound and the carbon material into camphene, and fully stirring for 2-10 h at the temperature of 50-100 ℃ to prepare slurry; wherein the solid content is 5-40 wt%;
(2) pouring the slurry prepared in the step (1) into a specific mould, quickly immersing the slurry into liquid nitrogen, taking out the slurry after 10min until the solvent is completely solidified; wherein the amount of the poured slurry is controlled to control the loading amount of sulfur to be 0.5-20mg/cm2；
(3) Vacuum drying the solidified body obtained in the step (2) for 6-24 hours in a low-temperature environment D to prepare a lamellar electrode;
(4) drying the thin-layer electrode prepared in the step (3) at room temperature to 100 ℃ for 2-24 hours to obtain a dried thin-layer electrode;
wherein the low-temperature environment D ranges from-200 ℃ to 40 ℃.
9. The method of claim 8, wherein:
when the low freezing point solvent is selected as water: in the step (1), the solid content is 20-30 wt%; the supporting capacity in the step (2) is 4-8mg/cm2；
When the low freezing point solvent is selected as camphene: in the step (1), the solid content is 20-30 wt%; in the step (2), the supporting capacity is 2-5mg/cm2。
10. Use of a laminar electrode according to any of claims 1 to 7, wherein: the lamellar electrode is used as a positive electrode in a lithium-sulfur battery.
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| KR20140062202A (en) * | 2012-11-14 | 2014-05-23 | 인하대학교 산학협력단 | Sulfur-doped graphene-based nanosheets for lithium-ion battery anodes |
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| KR20140062202A (en) * | 2012-11-14 | 2014-05-23 | 인하대학교 산학협력단 | Sulfur-doped graphene-based nanosheets for lithium-ion battery anodes |
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