CN109616649B - Positive electrode material of lithium-sulfur battery and preparation method thereof - Google Patents
Positive electrode material of lithium-sulfur battery and preparation method thereof Download PDFInfo
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Abstract
The invention provides a lithium-sulfur battery positive electrode material which comprises a base layer, a core layer positioned in the base layer, a first coating layer covering the base layer and a second coating layer covering the first coating layer, wherein the base layer is a mesoporous titanium dioxide layer, the core layer is a sulfur single layer, the first coating layer is a tungsten trioxide layer, and the second coating layer is a graphite particle layer. According to the lithium-sulfur battery positive electrode composite material provided by the invention, the tungsten trioxide layer and the graphite particle layer are respectively coated outside the mesoporous titanium dioxide layer, the physical limiting effect and the adsorption effect of chemical components of a one-dimensional pipeline of the mesoporous titanium dioxide can be simultaneously utilized, the problem of shuttle effect of intermediate product polysulfide ions generated in the charging and discharging processes of a lithium-sulfur battery positive electrode in the prior art is solved, the first discharge specific capacity of the lithium-sulfur battery positive electrode composite material prepared by the method is 759mAh/g under the multiplying power of 0.1C, and after 100 times of circulation, the circulation retention rate is up to 71.5%.
Description
Technical Field
The invention belongs to the technical field of battery materials, and particularly relates to a lithium-sulfur battery positive electrode material and a preparation method thereof.
Background
With the rapid development of new energy automobiles and mobile electronic devices, batteries with higher energy density are urgently needed. In a new energy system, a lithium-sulfur battery becomes one of the most potential secondary battery systems in the next generation due to the characteristics of high theoretical specific energy (2600W · h/kg), cheap elemental sulfur, environmental friendliness and the like.
Typical lithium sulfur batteries generally employ elemental sulfur as the positive electrodeAnd the metal lithium sheet is used as a negative electrode. However, lithium polysulfide, an intermediate product of the positive electrode of a lithium sulfur battery, has a shuttle effect, i.e., polysulfide (Li) generated from the positive electrode during charge and discharge2Sx) the intermediate is dissolved in the electrolyte, passes through the diaphragm, diffuses towards the negative electrode, and directly reacts with the lithium metal of the negative electrode, so that irreversible loss of effective substances in the battery, reduction of the service life of the battery and low coulombic efficiency are finally caused, and the commercialization of the lithium-sulfur battery is hindered.
Disclosure of Invention
In order to solve the problem of shuttle effect of lithium polysulfide, which is an intermediate product in a sulfur positive electrode of a lithium-sulfur battery in the prior art, the invention aims to provide a positive electrode material of the lithium-sulfur battery.
The invention also aims to provide a preparation method of the lithium-sulfur battery positive electrode material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the positive electrode material of the lithium-sulfur battery comprises a substrate layer, a core layer positioned in the substrate layer, a first coating layer for coating the substrate layer, and a second coating layer for coating the first coating layer;
the substrate layer is a mesoporous titanium dioxide layer, the core layer is a sulfur single layer, the first coating layer is a tungsten trioxide layer, and the second coating layer is a graphite particle layer.
Preferably, the graphite particles have a particle size of less than 50 nm.
The preparation method of the lithium-sulfur battery positive electrode material comprises the following steps:
(1) dispersing the mesoporous titanium dioxide and the tungsten trioxide in a solvent, and standing after ultrasonic oscillation;
(2) drying the product obtained in the step (1), adding the graphite particles, and uniformly mixing to obtain a semi-finished product;
(3) and (3) drying the semi-finished product obtained in the step (2), adding sublimed sulfur powder, uniformly mixing, placing in a tube furnace, and keeping the temperature at 200 ℃ under inert gas to obtain the lithium-sulfur battery cathode material.
Preferably, the mass ratio of the titanium dioxide to the tungsten trioxide in the step (1) is 1: (5-10).
Preferably, the solvent in step (1) is sodium lauryl sulfate.
Preferably, the time of the ultrasonic oscillation in the step (1) is 24-48 h.
Preferably, the drying standard in the step (2) is that the water content in the product is 20-35%.
Preferably, the mass ratio of the semi-finished product to the sublimed sulfur powder in the step (3) is 1: (15-20).
Preferably, the heat preservation time in the step (3) is 24-36 h.
Preferably, the inert gas in step (3) is argon.
The invention has the advantages of
1. According to the lithium-sulfur battery positive electrode material provided by the invention, the tungsten trioxide layer and the graphite particle layer are respectively coated outside the mesoporous titanium dioxide layer, so that the physical limitation effect and the chemical component adsorption effect of a one-dimensional pipeline of the mesoporous titanium dioxide can be simultaneously utilized, and the problem of shuttle effect of intermediate product polysulfide ions generated in the charging and discharging processes of the lithium-sulfur battery positive electrode in the prior art is solved;
2. the lithium-sulfur battery positive electrode material prepared by the method has the first discharge specific capacity of 759mAh/g under the multiplying power of 0.1C, and after 100 cycles, the cycle retention rate is as high as 71.5%.
Detailed Description
The following are specific examples of the present invention, and the technical solutions of the present invention will be further described with reference to the examples, but the present invention is not limited to the examples.
Example 1
The positive electrode material of the lithium-sulfur battery comprises a substrate layer, a core layer positioned in the substrate layer, a first coating layer for coating the substrate layer, and a second coating layer for coating the first coating layer;
the substrate layer is a mesoporous titanium dioxide layer, the core layer is a sulfur single layer, the first coating layer is a tungsten trioxide layer, the second coating layer is a graphite particle layer, and the particle size of the graphite particles is smaller than 50 nm.
Example 2
The preparation method of the lithium-sulfur battery positive electrode material comprises the following steps:
(1) dispersing the mesoporous titanium dioxide and the tungsten trioxide in a solvent, and standing after ultrasonic oscillation;
(2) drying the product obtained in the step (1), adding the graphite particles, and uniformly mixing to obtain a semi-finished product;
(3) and (3) drying the semi-finished product obtained in the step (2), adding sublimed sulfur powder, uniformly mixing, placing in a tube furnace, and keeping the temperature at 200 ℃ under inert gas to obtain the lithium-sulfur battery cathode material.
The mass ratio of the titanium dioxide to the tungsten trioxide in the step (1) is 1: 5, the solvent is sodium dodecyl sulfate, and the time of ultrasonic oscillation is 24 hours.
The drying standard in the step (2) is that the water content in the product is 20%, and the mass ratio of the semi-finished product to the sublimed sulfur powder is 1: 15.
and (3) keeping the temperature for 24 hours, wherein the inert gas is argon.
Example 3
The preparation method of the lithium-sulfur battery positive electrode material comprises the following steps:
(1) dispersing the mesoporous titanium dioxide and the tungsten trioxide in a solvent, and standing after ultrasonic oscillation;
(2) drying the product obtained in the step (1), adding the graphite particles, and uniformly mixing to obtain a semi-finished product;
(3) and (3) drying the semi-finished product obtained in the step (2), adding sublimed sulfur powder, uniformly mixing, placing in a tube furnace, and keeping the temperature at 200 ℃ under inert gas to obtain the lithium-sulfur battery cathode material.
The mass ratio of the titanium dioxide to the tungsten trioxide in the step (1) is 1: 10, the solvent is sodium dodecyl sulfate, and the time of ultrasonic oscillation is 48 h.
The drying standard in the step (2) is that the water content in the product is 35 percent, and the mass ratio of the semi-finished product to the sublimed sulfur powder is 1: 20.
and (3) keeping the temperature for 36h, wherein the inert gas is argon.
Example 4
The preparation method of the lithium-sulfur battery positive electrode material comprises the following steps:
(1) dispersing the mesoporous titanium dioxide and the tungsten trioxide in a solvent, and standing after ultrasonic oscillation;
(2) drying the product obtained in the step (1), adding the graphite particles, and uniformly mixing to obtain a semi-finished product;
(3) and (3) drying the semi-finished product obtained in the step (2), adding sublimed sulfur powder, uniformly mixing, placing in a tube furnace, and keeping the temperature at 200 ℃ under inert gas to obtain the lithium-sulfur battery cathode material.
The mass ratio of the titanium dioxide to the tungsten trioxide in the step (1) is 1: 7, the solvent is sodium dodecyl sulfate, and the time of ultrasonic oscillation is 36 h.
The drying standard in the step (2) is that the water content in the product is 27%, and the mass ratio of the semi-finished product to the sublimed sulfur powder is 1: 17.
and (3) keeping the temperature for 30h, wherein the inert gas is argon.
Comparative example 1
The preparation method of the lithium-sulfur battery positive electrode material comprises the following steps:
(1) dispersing the mesoporous titanium dioxide and the tungsten trioxide in a solvent, and standing after ultrasonic oscillation;
(2) drying the product obtained in the step (1), adding the graphite particles, and uniformly mixing to obtain a semi-finished product;
(3) and (3) drying the semi-finished product obtained in the step (2), adding sublimed sulfur powder, uniformly mixing, placing in a tube furnace, and keeping the temperature at 200 ℃ under inert gas to obtain the lithium-sulfur battery cathode material.
The mass ratio of the titanium dioxide to the tungsten trioxide in the step (1) is 1: 5, the solvent is sodium dodecyl sulfate, and the time of ultrasonic oscillation is 12 h.
The drying standard in the step (2) is that the water content in the product is 20%, and the mass ratio of the semi-finished product to the sublimed sulfur powder is 1: 15.
and (3) keeping the temperature for 24 hours, wherein the inert gas is argon.
Comparative example 2
The preparation method of the lithium-sulfur battery positive electrode material comprises the following steps:
(1) dispersing the mesoporous titanium dioxide and the tungsten trioxide in a solvent, and standing after ultrasonic oscillation;
(2) drying the product obtained in the step (1), adding the graphite particles, and uniformly mixing to obtain a semi-finished product;
(3) and (3) drying the semi-finished product obtained in the step (2), adding sublimed sulfur powder, uniformly mixing, placing in a tube furnace, and keeping the temperature at 200 ℃ under inert gas to obtain the lithium-sulfur battery cathode material.
The mass ratio of the titanium dioxide to the tungsten trioxide in the step (1) is 1: 2, the solvent is sodium dodecyl sulfate, and the time of ultrasonic oscillation is 24 hours.
The drying standard in the step (2) is that the water content in the product is 20%, and the mass ratio of the semi-finished product to the sublimed sulfur powder is 1: 15.
and (3) keeping the temperature for 24 hours, wherein the inert gas is argon.
Comparative example 3
The preparation method of the lithium-sulfur battery positive electrode material comprises the following steps:
(1) dispersing the mesoporous titanium dioxide and the tungsten trioxide in a solvent, and standing after ultrasonic oscillation;
(2) drying the product obtained in the step (1), adding the graphite particles, and uniformly mixing to obtain a semi-finished product;
(3) and (3) drying the semi-finished product obtained in the step (2), adding sublimed sulfur powder, uniformly mixing, placing in a tube furnace, and keeping the temperature at 200 ℃ under inert gas to obtain the lithium-sulfur battery cathode material.
The mass ratio of the titanium dioxide to the tungsten trioxide in the step (1) is 1: 5, the solvent is sodium dodecyl sulfate, and the time of ultrasonic oscillation is 24 hours.
The drying standard in the step (2) is that the water content in the product is 10%, and the mass ratio of the semi-finished product to the sublimed sulfur powder is 1: 15.
and (3) keeping the temperature for 24 hours, wherein the inert gas is argon.
Example of detection
Four lithium-sulfur battery positive electrode materials were prepared by the methods of example 3 and comparative examples 1 to 3, and the positive electrode materials were prepared into four battery positive electrode sheets numbered correspondingly.
Pairing the positive plate of the battery with lithium metal, adopting a Celgard diaphragm and adding 1mol L of lithium metal-1LiTFSI/(DOL+DME)(V/V＝1:1)/1％LiNO3The electrolyte is assembled into a battery to be tested for multiplying power and cycle performance. The results are shown in Table 1.
TABLE 1 Battery test data
According to the lithium-sulfur battery positive electrode composite material provided by the invention, the tungsten trioxide layer and the graphite particle layer are respectively coated outside the mesoporous titanium dioxide layer, the physical limiting effect and the adsorption effect of chemical components of a one-dimensional pipeline of the mesoporous titanium dioxide can be simultaneously utilized, the problem of shuttle effect of intermediate product polysulfide ions generated in the charging and discharging processes of a lithium-sulfur battery positive electrode in the prior art is solved, the first discharge specific capacity of the lithium-sulfur battery positive electrode composite material prepared by the method is 759mAh/g under the multiplying power of 0.1C, and after 100 times of circulation, the circulation retention rate is up to 71.5%.
The foregoing detailed description has described the principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the above-described embodiments, and variations and modifications of the present invention may be made without departing from the spirit and scope of the invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. The positive electrode material of the lithium-sulfur battery is characterized by comprising a substrate layer, a core layer positioned in the substrate layer, a first coating layer for coating the substrate layer, and a second coating layer for coating the first coating layer;
the substrate layer is a mesoporous titanium dioxide layer, the core layer is a sulfur single layer, the first coating layer is a tungsten trioxide layer, and the second coating layer is a graphite particle layer;
the preparation method of the lithium-sulfur battery positive electrode material comprises the following steps:
(1) dispersing mesoporous titanium dioxide and tungsten trioxide in a solvent, and standing after ultrasonic oscillation;
(2) drying the product obtained in the step (1), adding graphite particles, and uniformly mixing to obtain a semi-finished product;
(3) and (3) drying the semi-finished product obtained in the step (2), adding sublimed sulfur powder, uniformly mixing, placing in a tube furnace, and keeping the temperature at 200 ℃ under inert gas to obtain the lithium-sulfur battery cathode material.
2. The lithium sulfur battery positive electrode material of claim 1, wherein the graphite particles have a particle size of less than 50 nm.
3. The lithium-sulfur battery cathode material as claimed in claim 1, wherein the mass ratio of the mesoporous titanium dioxide to the tungsten trioxide in step (1) is 1 (5-10).
4. The positive electrode material for a lithium-sulfur battery according to claim 1, wherein the solvent in step (1) is sodium dodecyl sulfate.
5. The positive electrode material for the lithium-sulfur battery as claimed in claim 1, wherein the time of the ultrasonic vibration in the step (1) is 24-48 h.
6. The positive electrode material for the lithium-sulfur battery as claimed in claim 1, wherein the mass ratio of the semi-finished product in the step (3) to the sublimed sulfur powder is 1 (15-20).
7. The positive electrode material for the lithium-sulfur battery as defined in claim 1, wherein the heat preservation time in step (3) is 24-36 hours.
8. The positive electrode material for a lithium-sulfur battery according to claim 1, wherein the inert gas in step (3) is argon gas.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9012096B2 (en) * | 2004-05-28 | 2015-04-21 | Uchicago Argonne, Llc | Long life lithium batteries with stabilized electrodes |
| CN105609776A (en) * | 2016-02-21 | 2016-05-25 | 钟玲珑 | Preparation method for graphene/titanium dioxide hollow sphere/sulfur composite material |
| CN108172797A (en) * | 2017-12-27 | 2018-06-15 | 肇庆市华师大光电产业研究院 | A kind of preparation method of lithium sulfur battery anode material |
| CN108807947A (en) * | 2018-08-07 | 2018-11-13 | 河源广工大协同创新研究院 | A kind of preparation method of lithium sulfur battery anode material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9012096B2 (en) * | 2004-05-28 | 2015-04-21 | Uchicago Argonne, Llc | Long life lithium batteries with stabilized electrodes |
| CN105609776A (en) * | 2016-02-21 | 2016-05-25 | 钟玲珑 | Preparation method for graphene/titanium dioxide hollow sphere/sulfur composite material |
| CN108172797A (en) * | 2017-12-27 | 2018-06-15 | 肇庆市华师大光电产业研究院 | A kind of preparation method of lithium sulfur battery anode material |
| CN108807947A (en) * | 2018-08-07 | 2018-11-13 | 河源广工大协同创新研究院 | A kind of preparation method of lithium sulfur battery anode material |
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