CN109309217B - Preparation method of lithium-sulfur battery positive electrode material - Google Patents
Preparation method of lithium-sulfur battery positive electrode material Download PDFInfo
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- CN109309217B CN109309217B CN201810948717.7A CN201810948717A CN109309217B CN 109309217 B CN109309217 B CN 109309217B CN 201810948717 A CN201810948717 A CN 201810948717A CN 109309217 B CN109309217 B CN 109309217B
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H01M4/02—Electrodes composed of, or comprising, active material
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Abstract
The invention relates to a preparation method of a lithium-sulfur battery positive electrode material. Firstly, dispersing a graphene/carbon nanotube mixture into deionized water in an ultrasonic oscillation mode; and adding potassium permanganate and hydrochloric acid into the dispersion liquid, performing hydrothermal reaction, uniformly attaching manganous-manganic oxide nanosheets to the surface of the graphene/carbon nanotube, and finally, uniformly distributing sulfur nanoparticles on the surface of the graphene/carbon nanotube @ Mn3O4 composite material by a melting diffusion method to obtain the graphene/carbon nanotube @ Mn3O4@ S composite material. The composite material has the advantages of large specific surface area, porous structure and high conductivity when being used as a lithium sulfur battery anode material, can obviously improve the rate capability of the anode material when being applied to the lithium sulfur battery, and effectively solves the problem of too fast capacity attenuation in the electrode reaction process. The method is simple and easy to implement and is very suitable for engineering production.
Description
Technical Field
The invention relates to a preparation method of a lithium-sulfur battery positive electrode material, and particularly relates to a preparation method of a graphene/carbon nanotube @ Mn3O4@ S composite material.
Background
The theoretical specific energy of the lithium-sulfur battery is 2600WhKg < -1 >, which is 5 times of the theoretical specific energy (500WhKg < -1 >) of the current lithium ion battery, and is known as the most promising lithium secondary battery of the next generation. Is expected to be widely applied in the fields of portable electronic products, electric automobiles, aerospace crafts, power grid transmission and the like, plays a great role in the development of the current society, economy and science and technology, and has very bright application prospect.
However, under the room temperature condition, elemental sulfur has low conductivity, and soluble polysulfide is generated in the charging and discharging processes of the lithium-sulfur battery, so that various side reactions and volume changes are caused, and the utilization rate of active substances of the positive electrode of the lithium-sulfur battery is low, the rate performance is poor, and the cycle life is short, thereby restricting the development of the sulfur as the positive electrode material battery of the lithium secondary battery. Therefore, the improvement of the utilization rate and cycle life of the positive active material of the lithium-sulfur battery becomes an important development direction of the lithium-sulfur battery in the future.
Graphene is a novel two-dimensional nanomaterial, a nanosheet of the graphene is a two-dimensional nanomaterial with a single atomic layer thickness consisting of sp2 hybridized carbon atoms, the nanosheet is the thinnest and hardest nanomaterial known in the world, the strength of the nanomaterial is as high as 1.01Tpa, the strength of the nanomaterial is 100 times that of structural steel, and the density of the nanomaterial is 1/5 times that of the structural steel. The thermal conductivity coefficient is as high as 5300W/mK, higher than that of carbon nano tube and diamond, the electron mobility is over 200000cm 2/V.S at normal temperature, higher than that of carbon nano tube or silicon crystal, the resistivity is only about 1 omega.m, lower than that of copper or silver, and the material with the smallest resistivity in the world is obtained. The carbon nano tube is used as a one-dimensional nano material and has excellent conductive performance. The graphene/carbon nanotube hybrid material organically combines graphene and carbon nanotubes together in a covalent bond mode. The stacking phenomenon of the graphene can be prevented, the three-dimensional conductive network is formed, and the conductivity of the composite material is greatly improved.
The graphene/carbon nanotube hybrid material has very high conductivity, and when the graphene/carbon nanotube hybrid material is used as a lithium-sulfur battery anode material, the problem of non-conductivity of sulfur elements can be solved, and the conductivity of the anode material is improved. Due to the toughness and strength of the graphene/carbon nanotube hybrid material, the graphene is used as the framework of the positive electrode material of the lithium-sulfur battery, so that the problem of volume change of the positive electrode material of the lithium-sulfur battery can be effectively solved. However, carbon materials are themselves non-polar materials and have limited contribution to fixing polysulfides. Since the metal oxide represented by Mn3O4 is a polar material, and has a strong chemical action with polysulfide, the metal oxide can effectively adsorb the polysulfide, so that the graphene/carbon nanotube @ Mn3O4 composite material becomes an ideal framework of the positive electrode material of the lithium-sulfur battery.
Disclosure of Invention
The purpose of the invention is: the invention aims to provide a preparation method of a graphene/carbon nanotube @ Mn3O4 composite material aiming at the problems of the existing lithium-sulfur battery cathode material. According to the method, Mn3O4 precipitate is generated through an oxidation-reduction reaction between potassium permanganate and a carbon material in a coprecipitation reaction mode and is attached to the surface of the carbon material to form the graphene/carbon nanotube @ Mn3O4 composite material, so that various problems of a lithium-sulfur battery anode material are solved.
The technical scheme of the invention is as follows:
a preparation method of a lithium-sulfur battery positive electrode material is provided, which comprises the following steps:
preparation of graphene/carbon nanotube @ Mn3O4 composite material
Dispersing a graphene/carbon nanotube material in deionized water, and performing ultrasonic dispersion for 30min to obtain a graphene/carbon nanotube dispersion liquid, wherein the concentration of graphene/carbon nanotubes in the dispersion liquid is 0.1-5.0 mg/ml;
step two, respectively dissolving potassium permanganate and hydrochloric acid in the dispersion liquid, and uniformly stirring for 30 min;
transferring the dispersion liquid into a reaction kettle for heating, wherein the heating temperature is 200-300 ℃, and the heating time is 30-90 min;
step four, repeatedly cleaning the graphene/carbon nano tube @ Mn3O4 rechecked material by using absolute ethyl alcohol by using a vacuum filtration method, and drying the graphene/carbon nano tube @ Mn3O4 rechecked material in a vacuum drying furnace at the drying temperature of 60-80 ℃ for 18-24 h;
fifthly, roasting the dried composite material in an argon protection environment at the roasting temperature of 350-500 ℃ for 1-4 h;
preparation of graphene/carbon nanotube @ Mn3O4@ S composite material
Mixing the graphene/carbon nanotube @ Mn3O4 composite material and sublimed sulfur powder, and then filling the mixture into a sealed container, wherein the mass ratio of the graphene/carbon nanotube @ Mn3O4 composite material to the sublimed sulfur powder is 1: 1-1: 9;
and step seven, heating the sealed container in a drying furnace at the temperature of 150-165 ℃ for 12-24 hours.
Further, the graphene is in a folded sheet shape, the thickness of the sheet is 2-5 nm, the carbon nano tube is a single-walled carbon nano tube, the thickness of the Mn3O4 nano sheet is 1-4 nm, and the diameter of the sulfur particle is 5-20 nm.
Further, the uniform stirring is performed by a magnetic stirring apparatus.
By the method, Mn3O4 and S particles are uniformly distributed on the surface of the carbon material, the process is simple, the preparation of the graphene/carbon nanotube @ Mn3O4@ S composite material in large batch is easy to realize, and the engineering application is facilitated.
The invention has the advantages that: the invention realizes the rapid and accurate positioning during the processing of the composite material forming die frame and the template combined blank, does not need manual repair and polishing after the processing is finished, and improves the product quality and the production efficiency.
Drawings
FIG. 1 is a photograph of a transmission of the graphene/carbon nanotube @ Mn3O4@ S composite of FIG. 1.
Detailed Description
The present invention is described in further detail below.
Example 1:
the method for preparing the graphene/carbon nanotube @ Mn3O4@ S composite material comprises the following steps:
step one, dispersing 10mg of graphene/carbon nanotube hybrid material in 40ml of deionized water, and performing ultrasonic dispersion for 30min to obtain graphene/carbon nanotube dispersion liquid with the concentration of 0.25 mg/ml;
step two, dissolving 200mg of potassium permanganate and 0.14ml (with the concentration of 37%) of hydrochloric acid in the dispersion liquid in the step one, and reducing the magnetic force by half for 30 min;
step three, filling the dispersion liquid into a reaction kettle, and carrying out hydrothermal reaction for 2 hours at the temperature of 200 ℃;
step four, adopting a vacuum filtration method, repeatedly cleaning the graphene/carbon nano tube @ Mn3O4 rechecking material by using absolute ethyl alcohol, and drying the rechecking material in a vacuum drying furnace at the drying temperature of 80 ℃ for 24 hours;
fifthly, roasting the composite material for 3 hours at 400 ℃ under the protection of argon;
mixing the graphene/carbon nano tube @ Mn3O4@ S composite material with sublimed sulfur powder, and filling the mixture into a sealed container, wherein the mass ratio of the composite material to the sulfur powder is 1: 3;
and step six, heating the sealed container in a drying furnace at the heating temperature of 155 ℃ for 12 h.
Claims (3)
1. A preparation method of a lithium-sulfur battery positive electrode material is characterized by comprising the following steps: the method comprises the following steps:
preparation of graphene/carbon nanotube @ Mn3O4 composite material
Dispersing a graphene/carbon nanotube material in deionized water, and performing ultrasonic dispersion for 30min to obtain a graphene/carbon nanotube dispersion liquid, wherein the concentration of graphene/carbon nanotubes in the dispersion liquid is 0.1-5.0 mg/ml;
step two, respectively dissolving potassium permanganate and hydrochloric acid in the dispersion liquid, and uniformly stirring for 30 min;
transferring the dispersion liquid into a reaction kettle for heating, wherein the heating temperature is 200-300 ℃, and the heating time is 30-90 min;
step four, repeatedly cleaning the graphene/carbon nano tube @ Mn3O4 composite material by using absolute ethyl alcohol by using a vacuum filtration method, and drying the graphene/carbon nano tube @ Mn3O4 composite material in a vacuum drying furnace at the drying temperature of 60-80 ℃ for 18-24 hours;
fifthly, roasting the dried composite material in an argon protection environment at the roasting temperature of 350-500 ℃ for 1-4 h;
preparation of graphene/carbon nanotube @ Mn3O4@ S composite material
Mixing the graphene/carbon nanotube @ Mn3O4 composite material and sublimed sulfur powder, and then filling the mixture into a sealed container, wherein the mass ratio of the graphene/carbon nanotube @ Mn3O4 composite material to the sublimed sulfur powder is 1: 1-1: 9;
and step seven, heating the sealed container in a drying furnace at the temperature of 150-165 ℃ for 12-24 hours.
2. The method of claim 1, wherein the method comprises the steps of: the graphene is in a folded sheet shape, the thickness of the sheet is 2-5 nm, the carbon nano tube is a single-walled carbon nano tube, the thickness of the Mn3O4 nano sheet is 1-4 nm, and the diameter of sulfur particles is 5-20 nm.
3. The method of claim 1, wherein the method comprises the steps of: the homogeneous stirring is carried out by means of a magnetic stirring apparatus.
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