CN111900407B - Lithium-sulfur battery positive electrode material and preparation method thereof - Google Patents

Lithium-sulfur battery positive electrode material and preparation method thereof Download PDF

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CN111900407B
CN111900407B CN202010772098.8A CN202010772098A CN111900407B CN 111900407 B CN111900407 B CN 111900407B CN 202010772098 A CN202010772098 A CN 202010772098A CN 111900407 B CN111900407 B CN 111900407B
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lithium
pan
positive electrode
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sulfur battery
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CN111900407A (en
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贺高红
李祥村
周长宇
姜晓滨
姜福林
郑文姬
张悦
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Dalian University of Technology
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/626—Metals
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention relates to a lithium-sulfur battery positive electrode material and a preparation method thereof, in particular to Fe3The preparation process of the C nanoparticle-doped fiber carbon-based lithium-sulfur battery anode material with the hollow vesicle structure comprises the steps of firstly preparing ferric oxide nanoparticles with regular shapes, then uniformly and properly coating the particles into silk threads by using an electrostatic spinning method, and then carrying out pre-oxidation and carbonization on the silk threads to finish the preparation, wherein the particle size of Fe in the carbonization process is 140-750nm2O3Pulverizing into fine Fe with particle diameter of 5-10nm3C nanoparticles and leaving hollow vesicles. The material designed by the invention is Fe3The chemical adsorption effect of the carbon fiber is combined with the physical limitation of the hollow vesicles of the carbon fiber, polysulfide is adsorbed and fixed, a limited space is provided, a good ion and electron transmission path is further guaranteed, the volume expansion of charge and discharge is relieved, the conductivity of the material is improved by the doped N atoms, and the overall electrochemical performance of the Li-S battery is improved.

Description

Lithium-sulfur battery positive electrode material and preparation method thereof
Technical Field
The invention belongs to the technical field of battery energy storage materials, and particularly relates to a lithium-sulfur battery positive electrode material and a preparation method thereof.
Background
The global warming and the reduction of the traditional energy have led scientists to pay attention to the utilization efficiency of the traditional energy and the development and utilization of new energy. Researchers are concerned not only with clean and renewable energy sources, but also with advanced energy storage. Therefore, the development of high performance electrochemical energy storage devicesHas become one of the important issues of the energy strategy project established by governments of various countries in the world. With the social progress and economic development, and the demand of people for green energy and the awareness of protecting the ecological environment are further enhanced, a secondary battery represented by a lithium ion battery is used as a convenient and recyclable energy storage device and is widely applied to the aspects of mobile phones, notebook computers, digital cameras, electric bicycles and the like. The advantages of the lithium ion secondary battery system are the following: the battery has the advantages of high specific energy, high working voltage, long cycle life, small self-discharge and no environmental pollution, and is called a green battery. However, with the continuous progress of society, electronic equipment continues to be developed in a direction of lightness and thinness, and energy crisis is becoming more serious, new energy electric vehicles become targets of all countries in the world, and the development of the new energy electric vehicles puts higher requirements on the energy density of secondary batteries, particularly in the field of electric vehicles, when the distance operation is more than 500km, the energy density of required batteries is more than 550Wh/kg, and the development target in the period of 'thirteen five' in China requires that the specific energy of a single battery reaches 300 Wh/kg-1But commercially used LiFeO4、LiCoO2And LiNi1/3Co1/3Mn1/3O2The theoretical capacity of the equal positive electrode material is not more than 300 Wh/kg-1It is difficult to meet the requirement of electric vehicles for high specific energy batteries, and therefore, the development of a new generation of high theoretical energy secondary battery system is the focus of current research. In a new secondary battery system, lithium-sulfur batteries are based on 16Li + S8＝8Li2S is the oxidation-reduction reaction, metal lithium is used as a negative electrode, elemental sulfur is used as an active substance of the positive electrode, and the theoretical specific capacity of the lithium ion battery is 1672 mAh.g-1Theoretical energy density is as high as 2600 Wh.kg-1The energy density of the lithium ion battery is 5 times of the theoretical energy density of the lithium ion battery, natural resources of elemental sulfur are very rich, the elemental sulfur is a byproduct of coal chemical industry, the price is low, the environment is friendly, and the like, and the lithium sulfur battery has a great application prospect based on the advantages. At present, the theoretical energy density of a lithium ion battery cannot meet the requirements of people, and several factors which hinder the development of the lithium ion battery mainly exist, such as: (1) elemental sulfur and its products are insulating materials, which in turn affect lithium sulfurThe conductivity of the battery. (2) In the charge-discharge cycle process of the lithium-sulfur battery, due to the different densities of elemental sulfur and lithium sulfide which is a product of the elemental sulfur, severe volume expansion can be caused, and the normal work of an electrode is influenced, so that the cycle service life of the lithium-sulfur battery is influenced. (3) In the discharging process, the chemical reaction of the metal lithium and the elemental sulfur is a multi-step reaction, a lithium polysulfide intermediate is generated in the reaction process, soluble lithium polysulfide can be dissolved in the organic electrolyte, the lithium polysulfide leaves the positive electrode under the action of concentration difference, the utilization rate of active substances is low, and when the lithium polysulfide passes through the diaphragm and moves to the negative electrode, part of the lithium polysulfide reacts with the metal lithium to generate lithium sulfide, so that the self-discharging phenomenon is generated. And during charging, under the action of voltage, another part of lithium polysulfide leaves the negative electrode and moves back to the positive electrode through the separator again, and the process is repeated to generate the shuttle effect. Therefore, in the current stage, a new type of cathode material is sought, the problem of fast capacity fading of the lithium-sulfur battery is solved, and the structure and function design of the material can be performed through the following aspects: (1) the electronic rapid transmission is realized by relying on a conductive network; (2) a large specific surface area is utilized to provide sulfur loading sites; (3) a proper pore structure is designed in a microstructure, so that the influence of lithium deposition is weakened; (4) the surface performance of the material is improved, and the material composition can be further optimized by methods such as atom doping and the like.
Disclosure of Invention
The invention aims to provide a lithium-sulfur battery positive electrode material which is formed by stacking a plurality of layers of carbon fiber spinning membranes with hollow vesicles and fine Fe with the particle size of 5-10nm3C, compounding the nano particles. The composite material is prepared by an electrostatic spinning method, composition and structure optimization is performed, the mass transfer process is regulated, the specific surface area and the adsorptivity are improved, the interface mass transfer resistance is reduced, the problems of volume expansion and the like in the charging and discharging of the battery are effectively relieved, and the electrochemical performance of the battery is improved.
The invention also aims to provide a preparation method of the lithium-sulfur battery anode material, which is simple and easy to implement, strong in operability, easy to produce in large scale, green and environment-friendly, and low in cost.
In order to achieve the above object, the present invention has the following technical means.
The lithium-sulfur battery positive electrode material is composed of a multi-layer stacked carbon fiber spinning membrane with hollow vesicles and fine Fe with the particle size of 5-10nm3C, compounding nano particles; said Fe3C nano particles are dispersed on the inner wall of the vesicle, and the Fe3The mass percentage of the C nano-particles in the anode material is 10-80%.
The invention relates to a preparation method of a lithium-sulfur battery anode material, which is prepared from alpha-Fe2O3Mixing the nano particles with PAN/PVP mixed spinning solution (polyacrylonitrile/polyvinylpyrrolidone mixed spinning solution), and performing electrostatic spinning on the alpha-Fe2O3Nano particles are uniformly coated into the filament, and the alpha-Fe2O3The particle size (grain diameter) is 140-750nm, and the nano-particles are prepared through pre-oxidation and carbonization processes; alpha-Fe with grain size of 140-750nm in the carbonization process2O3Pulverizing into fine Fe with particle diameter of 5-10nm3C nanoparticles and leaving hollow vesicles.
A preparation method of a lithium-sulfur battery positive electrode material specifically comprises the following steps:
(1) preparation of alpha-Fe with different morphologies2O3Template:
slowly adding NaOH solution into FeCl under mechanical stirring3To the solution, Na is then added2SO4Continuously stirring the solution uniformly, then sealing the reaction container, putting the reaction container into an oven for aging at the aging temperature of 60-140 ℃ for 1-12 days, taking out the solution after aging, cooling the solution to room temperature, washing the lower-layer red slurry-like solid with deionized water, and drying the solid to obtain the reddish brown alpha-Fe2O3Powder particles;
(2) preparing an N-doped PAN-coated iron oxide film by coaxial electrostatic spinning:
dissolving PAN and PVP in DMF to prepare PAN/PVP mixed spinning solution, and mixing alpha-Fe2O3Dissolving the powder in the mixed spinning solution to form suspension, performing electrostatic spinning, and sealing and storing to obtain N-doped PAN-coated alpha-Fe2O3A film.
(3) Pre-oxidation and carbonization film forming processes:
coating N-doped PAN with alpha-Fe2O3The film is placed in a muffle furnace for pre-oxidation, and is placed in a muffle furnace filled with Ar/N after natural cooling and temperature reduction2Carbonizing at 700-3A carbon fiber-based lithium-sulfur battery cathode material with a hollow vesicle structure doped with C nanoparticles).
The concentration of the NaOH solution adopted in the step (1) is 4-8mol/L, and FeCl is adopted3The concentration of the solution is 1-3 mol/L.
Na is adopted in the step (1)2SO4Adjusting the diameter and microscopic shape of iron oxide particles, Na2SO4The concentration of the solution is 0-1 mol/L.
In the step (1), the drying temperature is 40-200 ℃, and the drying time is 1-36 hours.
The average molecular weight of the PAN raw material adopted in the step (2) is 40000-250000, and the mass ratio of the PAN to the PVP raw material is 1:1-20: 1. Furthermore, the average molecular weight of the PAN raw material is 150000, and the mass ratio of the PAN to the PVP raw material is 3: 1.
The concentration of the PAN/PVP mixed spinning solution adopted in the step (2) is 0.05mol/L-0.6 mol/L. Further, the concentration of the PAN/PVP mixed spinning solution is 0.2 mol/L.
alpha-Fe added to the PAN/PVP mixed spinning solution in the step (2)2O3The addition amount of the particles is 100-600 mg/ml.
The electrostatic spinning in the step (2) is carried out at the temperature of 25 ℃ and the relative humidity of less than 40 percent.
The time of the pre-oxidation (oxygen-containing pre-oxidation) process in the step (3) is 1-3h, and the temperature is 120-320 ℃. Further, the time of the oxygen-containing pre-oxidation process is 2.5h, and the temperature is 250 ℃.
The invention also provides a lithium-sulfur battery, and the positive electrode material or the positive electrode carrier material of the battery adopts the positive electrode material of the lithium-sulfur battery.
The invention has the following beneficial effects: the invention provides a lithium-sulfur battery positive electrode material, and a lithium-sulfur battery positive electrodeFe in pole material3Precursor of C nanoparticles alpha-Fe2O3The nano particles can be uniformly and efficiently loaded in the high polymer yarn through an electrostatic spinning method, and a new method is provided for the design of an electrode structure. The material has abundant controllable pore channel structures and larger specific surface area, can physically adsorb polysulfide to a greater extent, and simultaneously promotes the redox kinetics of the polysulfide. Carbide Fe3The advantages and disadvantages of C and carbon structure are complemented, and Fe is added3The chemical adsorption effect of C is combined with the physical limitation of hollow vesicles of carbon fibers, polysulfide is adsorbed and fixed, a confined space is provided, a good ion and electron transmission path is further guaranteed, the volume expansion of charge and discharge is relieved, and the conductivity of the material is improved by the doped N atoms. Therefore, the high performance of the material as a battery material is ensured, and the aims of improving the cycle stability and the rate capability of the lithium-sulfur battery are finally fulfilled.
The invention provides a preparation method of a lithium-sulfur battery cathode material, which is simple and easy to obtain, low in price, green and environment-friendly, and suitable for industrial large-scale expanded preparation production.
Drawings
Fig. 1 is a scanning electron microscope image of a positive electrode material for a lithium sulfur battery prepared in example 1.
Fig. 2 is a transmission electron microscope image of the positive electrode material for a lithium sulfur battery prepared in example 1.
Fig. 3 is an energy dispersive X-ray spectroscopy chart of the lithium sulfur battery cathode material prepared in example 1.
Fig. 4 is a graph showing cycle performance of a lithium sulfur battery including the positive electrode material for a lithium sulfur battery prepared in example 1.
Detailed description of the preferred embodiments
The invention is further illustrated, but not limited, by the following examples.
In the following examples:
(1) scanning Electron Microscope (SEM) testing: the instrument model of the scanning electron microscope is Nova Nano SEM 450, FEI company, USA. The test sample and the preparation method are as follows: the lithium sulfur battery positive electrode material prepared in the example was dried to prepare a sample, and SEM test was performed.
(2) Energy dispersive X-ray spectroscopy (EDX) testing: the instrument model is Nova Nano SEM 450 from FEI company in USA. The test sample and the preparation method are as follows: the lithium-sulfur battery positive electrode material prepared in the example was dried to prepare a sample, and EDX test was performed.
(3) Testing the performance of the lithium-sulfur battery: using the instrument model lan CT2100A, wuhan blue electronics gmbh, test parameters: the charge-discharge voltage threshold is 1.7-2.8V, and the charge-discharge multiplying power is as follows: 0.1C, 0.2C, 0.5C, 1C, and 2C, charge and discharge temperature: at 25 ℃.
Example 1
Under mechanical stirring, 90mL of 6.0mol/L NaOH solution was slowly added to 100mL of 2.0mol/L FeCl3Stirring was continued for 10 minutes. The reaction vessel was then sealed and placed in an oven at 100 ℃ for constant temperature aging for 8 days. Taking out, cooling to room temperature, removing supernatant, washing lower layer red slurry solid with deionized water for 3 times, and drying at 60 deg.C for 12 hr to obtain red alpha-Fe2O3And (3) powder. Dissolving PAN and PVP with average molecular weight of 150000 in DMF at a mass ratio of 3:1 to prepare 100ml of 0.2g/ml PAN/PVP mixed spinning solution, and mixing the prepared alpha-Fe2O3Dissolving the particles in mixed spinning solution to form suspension, and dissolving alpha-Fe in PAN/PVP mixed spinning solution2O3The addition amount of the particles is 10g, electrostatic spinning is carried out at the temperature of 25 ℃ and the relative humidity is lower than 40%, and then sealing storage is carried out to obtain N-doped PAN-coated alpha-Fe2O3Film of alpha-Fe2O3The particle size was 500-700 nm. And (3) placing the film in a muffle furnace, pre-oxidizing for 120min at 250 ℃, naturally cooling, and cutting the shape (such as a round shape conforming to a battery test). Placing the pre-oxidized film in a tubular furnace environment filled with Ar gas, carbonizing at 800 ℃, and naturally cooling to obtain Fe3C nanoparticle-doped fiber carbon-based lithium-sulfur battery positive electrode material with hollow vesicle structure, Fe3The mass percentage of the C nanoparticles in the positive electrode material was 80%.
(1) And (3) testing by a scanning electron microscope:
the test results are shown in fig. 1 and fig. 2, the positive electrode material of the lithium-sulfur battery is in a regular threading thread shape, the thread has a hollow vesicle structure, and Fe is dispersed on the inner wall of the vesicle3And C, nano-particles. The specific surface of the cathode material is 101.6g/m2，Fe3The C nano-particles are 5-10 nm.
(2) Energy dispersive X-ray spectroscopy test:
the test results are shown in FIG. 3, and fine Fe with the particle size of 5-10nm exists in the interior of the silk in the positive electrode material of the lithium-sulfur battery3And C, nano particles, which proves that the nano particles are uniformly distributed in the spinning film, and the element distribution diagram also shows that nitrogen is doped in the material.
(3) Testing the electrochemical performance of the lithium-sulfur battery:
carrying out charge-discharge cycle test on the lithium-sulfur battery containing the cathode material, assembling the battery in a glove box, taking a lithium sheet as a cathode, taking Celgard 2325 as a diaphragm, taking the electrolyte as a non-aqueous phase electrolyte, adding 1% LiNO into a 1,3 epoxy pentalane/ethylene glycol dimethyl ether (volume ratio 1:1) solution containing 1M lithium bistrifluoromethylenesulfonamide (LiTFSI), and adding 1% LiNO3The additive of (1). The C/S composite slurry is coated on the anode material. As a result, as shown in FIG. 4, the sulfur loading was 1.5mg/cm2Under the condition of (1), the first-week discharge capacity can reach 1355mAh g at 0.1C-1The capacity can reach 1124mAh g in 0.2C discharge state-1The capacity can reach 0.5C:1008mAh g in the discharge state -11C, the capacity can reach 927mAh g in a discharge state-1The capacity can reach 795mAh g under the high-rate discharge 2C state-1. The discharge capacity after 0.5C circulation for 100 circles still reaches 1097.5mAh g-1The battery has excellent cycle stability.
The above example is only one of the specific implementation manners of the present invention, and the description thereof is more specific, but this should not be construed as limiting the scope of the present invention. It must be pointed out that several variants and extensions obvious to a person skilled in the art may be made without departing from the inventive concept, all falling within the scope of protection of the present invention.

Claims (8)

1. Lithium sulfurA battery positive electrode material, characterized in that: multilayer stacked carbon fiber spinning membrane with hollow vesicles and fine Fe with particle size of 5-10nm3C, compounding nano particles; said Fe3C nano particles are dispersed on the inner wall of the vesicle, and the Fe3The mass percentage of the C nano particles in the anode material is 10-80%; the lithium-sulfur battery positive electrode material consists ofα-Fe2O3Mixing the nano particles with PAN/PVP mixed spinning solution, and performing electrostatic spinningα-Fe2O3 The nano particles are uniformly coated into the silk threads and then are prepared through the pre-oxidation and carbonization processes; the grain diameter of 140-750nm Fe in the carbonization process2O3Pulverizing into fine Fe with particle diameter of 5-10nm3C nanoparticles and leaving hollow vesicles.
2. A method for preparing a positive electrode material for a lithium-sulfur battery according to claim 1, characterized in that: the method specifically comprises the following steps:
(1) preparation of different morphologiesα-Fe2O3Template:
slowly adding NaOH solution into FeCl under mechanical stirring3To the solution, Na is then added2SO4Continuously stirring the solution uniformly, then sealing the reaction container, putting the reaction container into an oven for aging at the aging temperature of 60-140 ℃ for 1-12 days, taking out the solution after aging, cooling the solution to room temperature, washing the lower-layer red slurry-like solid with deionized water, and drying the solid to obtain the reddish brownα-Fe2O3Powder;
(2) preparing an N-doped PAN-coated iron oxide film by coaxial electrostatic spinning:
dissolving PAN and PVP in DMF to prepare PAN/PVP mixed spinning solution, mixingα-Fe2O3Dissolving the powder in the mixed spinning solution to form suspension, performing electrostatic spinning, and sealing for storage to obtain N-doped PAN coatingα-Fe2O3The N element is derived from PAN polymer material;
(3) film forming and carbonizing processes:
coating N-doped PANα-Fe2O3Placing the film in a muffle furnace for pre-oxidation, naturally cooling, placing the pre-oxidized film in a muffle furnace filled with Ar/N2Carbonizing at the temperature of 700 plus 1000 ℃ in a gas tubular furnace environment, and naturally cooling to obtain the lithium-sulfur battery anode material.
3. The method of claim 2, wherein the method comprises the steps of: the concentration of the NaOH solution adopted in the step (1) is 4-8mol/L, and FeCl is adopted3 The concentration of the solution is 1-3 mol/L; na (Na)2SO4 The concentration of the solution is 0-1 mol/L.
4. The method of claim 2, wherein the method comprises the steps of: adding to PAN/PVP mixed spinning solution in step (2)α-Fe2O3 The addition amount of the particles is 100-600 mg/ml.
5. The method of claim 2, wherein the method comprises the steps of: the average molecular weight of the PAN raw material adopted in the step (2) is 40000-250000, and the mass ratio of the PAN to the PVP raw material is 1:1-20: 1.
6. The method of claim 2, wherein the method comprises the steps of: the concentration of the PAN/PVP mixed spinning solution adopted in the step (2) is 0.05mol/L-0.6 mol/L.
7. The method of claim 2, wherein the method comprises the steps of: the time of the pre-oxidation process in the step (3) is 1-3h, the temperature is 120-320 ℃, and the cooling rate of the pre-oxidation temperature to the room temperature is 1-10oC min-1。
8. A lithium sulfur battery characterized by: the positive electrode material or the positive electrode support material of the battery adopts the positive electrode material of the lithium-sulfur battery according to claim 1.
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