A kind of preparation method of lithium sulfide composite material coated with graphene/lithium titanate

A technology of lithium titanate coating and composite materials, which is applied in the direction of electrochemical generators, electrical components, battery electrodes, etc., can solve the problems of potential safety hazards, restrictions on the application of lithium-sulfur batteries, and failure of lithium-sulfur secondary batteries. Stable structure, improved electronic conductivity, and improved lithium ion mobility

Active Publication Date: 2018-08-14
苏州优越新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the lithium-sulfur battery system, since the sulfur-based positive electrode does not contain lithium, metal lithium needs to be used as the negative electrode to provide the lithium source. However, during the cycle, the metal lithium negative electrode is easy to generate lithium dendrites and pulverization on the surface, which not only poses a safety hazard. , and the consumption of electrolyte leads to premature failure of lithium-sulfur secondary batteries, which limits the application of lithium-sulfur batteries

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  • A kind of preparation method of lithium sulfide composite material coated with graphene/lithium titanate

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Experimental program
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Effect test

Embodiment 1

[0020] (1) Put commercial lithium sulfide into a sealed ball mill tank in an inert gas-protected glove box, and then put it into a ball mill for ball milling for 0.5 hours at a ball milling speed of 3000 rpm to obtain nanometer lithium sulfide.

[0021] (2) Add tetrabutyl titanate into ethanol under stirring, and dissolve to form a tetrabutyl titanate ethanol solution with a mass concentration of 10%.

[0022] (3) Disperse the obtained nano-lithium sulfide into the ethanol solution containing ammonia water, stir continuously to form a 10% 50ml suspension, in which the volume concentration of ammonia water is 5%, and then add 50ml tetrabutyl titanate ethanol solution dropwise into the suspension, stirred and reacted at 40°C for 48 hours, and then evaporated the solvent to obtain a solid powder, which was added to a muffle furnace protected by an inert gas for reaction, and reacted at 300°C for 3 hours to obtain a precursor.

[0023] (4) Mix the obtained precursor with lithium c...

Embodiment 2

[0026] (1) Put commercial lithium sulfide into a sealed ball mill tank in an inert gas-protected glove box, and then put it into a ball mill for 3 hours of ball milling at a milling speed of 500 rpm to obtain nanometer lithium sulfide.

[0027] (2) Add tetrabutyl titanate into ethanol under stirring, and dissolve to form a tetrabutyl titanate ethanol solution with a mass concentration of 5%.

[0028] (3) Disperse the obtained nano-lithium sulfide into the ethanol solution containing ammonia water, stir continuously to form a 5% 50ml suspension, wherein the volume concentration of ammonia water is 1%, and then add 5ml tetrabutyl titanate ethanol solution dropwise to In the suspension, stirred and reacted at 60°C for 24 hours, and then evaporated the solvent to obtain a solid powder, which was added to a muffle furnace protected by an inert gas for reaction, and reacted at 400°C for 1 hour to obtain a precursor.

[0029] (4) The obtained precursor was mixed with lithium carbonat...

Embodiment 3

[0032] (1) Put commercial lithium sulfide into a sealed ball mill tank in an inert gas-protected glove box, and then put it into a ball mill for ball milling for 1 hour at a ball milling speed of 2000 rpm to obtain nanometer lithium sulfide.

[0033] (2) Add tetrabutyl titanate into ethanol under stirring, and dissolve to form a tetrabutyl titanate ethanol solution with a mass concentration of 7%.

[0034] (3) Disperse the obtained nano-lithium sulfide into an ethanol solution containing ammonia water, stir continuously to form a 6% 50ml suspension, in which the volume concentration of ammonia water is 2%, and then add 10ml tetrabutyl titanate ethanol solution dropwise to In the suspension, stirred and reacted at 50°C for 36 hours, and then evaporated the solvent to obtain a solid powder, which was added to a muffle furnace protected by an inert gas for reaction, and reacted at 350°C for 2 hours to obtain a precursor.

[0035] (4) Mix the obtained precursor with lithium carbon...

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Abstract

The invention provides a preparation method for a graphene / lithium titanate coated lithium sulfide composite material. The preparation method comprises the following steps of (1) loading commercial lithium sulfide into a sealed ball milling tank; then putting the tank into a ball mill to be subjected to ball milling to obtain nanometer lithium sulfide; (2) adding tetrabutyl titanate to ethyl alcohol while stirring, and dissolving to form a tetrabutyl titanate ethyl alcohol solution; (3) enabling the nanometer lithium sulfide to be dispersed to an ethyl alcohol solution containing ammonium hydroxide, and adding the tetrabutyl titanate ethyl alcohol solution to a suspension liquid in a dropwise manner; (4) enabling an obtained precursor to be mixed with lithium carbonate powder, and adding the mixture to a muffle furnace under inert gas protection to perform a reaction to obtain the lithium titanate coated lithium sulfide; and (5) adding the lithium titanate coated lithium sulfide and graphene to tetrahydrofuran, and performing an ultrasonic reaction to obtain the graphene / lithium titanate coated lithium sulfide composite material. The lithium titanate structure is relatively stable in the charge-discharge process of the composite material, so that the loss of sulfur-based material can be effectively prevented.

Description

technical field [0001] The invention relates to the synthesis of nanometer materials, in particular to a preparation method of a cathode material of a lithium-sulfur battery. Background technique [0002] A lithium-sulfur battery is a battery system in which metallic lithium is used as the negative electrode and elemental sulfur is used as the positive electrode. Lithium-sulfur batteries have two discharge platforms (about 2.4 V and 2.1 V), but their electrochemical reaction mechanism is relatively complicated. Lithium-sulfur batteries have the advantages of high specific energy (2600 Wh / kg), high specific capacity (1675 mAh / g), and low cost, and are considered to be a promising new generation of batteries. However, at present, there are problems such as low utilization of active materials, low cycle life and poor safety, which seriously restrict the development of lithium-sulfur batteries. The main reasons for the above problems are as follows: (1) elemental sulfur is an ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/485H01M4/58H01M10/0525
CPCH01M4/366H01M4/485H01M4/5815H01M10/0525Y02E60/10
Inventor 钟玲珑肖丽芳
Owner 苏州优越新材料有限公司
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