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A kind of preparation method of nano sulfur particle
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A nano-sulfur and particle technology, applied in the preparation/purification of sulfur, nanotechnology, nanotechnology, etc., can solve the problems of affecting battery performance, reducing sulfur content, uneven dispersion of sulfur powder, etc. cost, good effect
Active Publication Date: 2018-04-03
GUANGDONG ZHUGUANG NEW ENERGY TECH
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However, elemental sulfur itself is not conductive, and must be combined with a conductive substance to make an electrode. Due to the introduction of a conductive agent as a conductive component, the sulfur content in the positive electrodecoating has been greatly reduced, thereby reducing the lithium-sulfur content. The energy density of the battery; at the same time, large particles of sulfur powder are often unevenly dispersed, which affects the performance of the battery; therefore, the use of small particle size (nanoscale) sulfur powder to prepare lithium-sulfur batteries is an effective solution
[0006] At present, the method of preparing nano-sulfur particles is high-temperature gas-phase solidification method, which needs to be carried out under the protection of high temperature and inert gas, and has high requirements on the production environment, so the manufactured nano-sulfur particles are very expensive
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Embodiment 1
[0027] Preparation of sulfur element solution: at 40°C, uniformly mix sulfur element with a particle size of 10 μm and carbon disulfide to obtain a sulfur carbon disulfide saturated solution for use;
[0028] Recrystallization: In the case of ultrasonic treatment, the above solution is cooled to 20°C at a rate of 1°C / min, so that the sulfur-containing elemental substance in the solution is precipitated, and a slurry containing nano-sulfur particles is obtained;
[0029] Drying: At 20°C, use filtration to separate the precipitated sulfur particles from the solution, and then dry them in a vacuum drying oven at 60°C to obtain massive sulfur particles;
[0030] Pulverization: the above-mentioned sulfur block is pulverized by ball milling process to obtain nanometer sulfur particles.
Embodiment 2
[0031] Embodiment 2, different from Embodiment 1, this embodiment includes the following steps:
[0032] Preparation of sulfur element solution: at 40°C, uniformly mix sulfur element with a particle size of 10 μm and carbon disulfide to obtain a sulfur carbon disulfide saturated solution for use;
[0033] Recrystallization: In the case of ultrasonic treatment, the above solution is cooled to 20°C at a rate of 1°C / min, so that the sulfur-containing elemental substance in the solution is precipitated, and a slurry containing nano-sulfur particles is obtained;
[0034] Drying: At 20°C, use centrifugation to separate the above-mentioned precipitated sulfur elemental particles from the solution, then place them in a freeze dryer for freeze-drying, and remove the solvent to obtain massive sulfur particles;
[0035] Pulverization: the above-mentioned sulfur block is pulverized by ball milling process to obtain nanometer sulfur particles.
[0036] Others are the same as in Example 1,...
Embodiment 3
[0037] Embodiment 3, different from Embodiment 1, this embodiment includes the following steps:
[0038] Preparation of sulfur element solution: at 40°C, uniformly mix sulfur element with a particle size of 10 μm and carbon disulfide to obtain a sulfur carbon disulfide saturated solution for use;
[0039] Recrystallization: In the case of ultrasonic treatment, the above solution is cooled to 20°C at a rate of 0.1°C / min, so that the sulfur-containing elemental substance in the solution is precipitated, and a slurry containing nano-sulfur particles is obtained;
[0040] Drying: At 20°C, use filtration to separate the precipitated sulfur particles from the solution, and then dry them in a vacuum drying oven at 60°C to obtain massive sulfur particles;
[0041] Pulverization: the above-mentioned sulfur block is pulverized by ball milling process to obtain nanometer sulfur particles.
[0042] Others are the same as in Example 1, and will not be repeated here.
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Abstract
The invention belongs to the field of a lithiumsulfur battery, and in particular relates to a preparation method for nanometer sulfur particles. The preparation method comprises four steps of preparation of a sulfur elementary substance solution, recrystallization, drying and smashing; a sulfur saturated solution at the temperature of T1 is prepared firstly; then the temperature of the saturated solution is reduced to be T2 (T2 is less than T1) to enable sulfur to be gradually separated out to obtain the nanometer sulfur particles; in the process, the temperature reduction speed and the T2-T1 value can be controlled, disturbance factors (stirring, ultrasonic and the like) can be added or a nucleating agent and the like can be introduced, so that the particle size of the separated out sulfur particles is controlled, and the finally-obtained particle size is the nanoscale sulfur particle; the temperature T2 is kept, and the nanometer particles are separated from the solution by means of filtering, centrifuging and the like; then the particles are dried (freezing, vacuum drying and the like; the granules are not agglomerated under freezing and drying along with a better effect), and then the particles are smashed by simple ball milling or smashed mechanically to obtain the nanometer sulfur particles. The process is simple and easy to implement, and a large batch of nanometer sulfur particles can be prepared at low cost.
Description
technical field [0001] The invention belongs to the field of lithium-sulfur batteries, and in particular relates to a preparation method of nanometer sulfur particles. Background technique [0002] Since 1991, carbon materials were creatively used in the field of lithium-ion batteries and brought about revolutionary changes in this field, that is, after multiple charging and discharging efficiently and safely, they have been widely used in mobile phones, cameras, and notebooks. computers and other portable appliances. Compared with traditional lead-acid, Ni-Cd, MH-Ni batteries, lithium-ion batteries have higher specific volumeenergy density, specific gravimetric energy density, better environmental friendliness, smaller self-discharge and longer battery life. It is an ideal power supply for mobile appliances, power supplies for electric vehicles, and storage appliances for power stations in the 21st century. [0003] However, with the improvement of life taste, people put...
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