CN110783537A - Polypyrrole lithium-sulfur battery material - Google Patents
Polypyrrole lithium-sulfur battery material Download PDFInfo
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- CN110783537A CN110783537A CN201910886264.4A CN201910886264A CN110783537A CN 110783537 A CN110783537 A CN 110783537A CN 201910886264 A CN201910886264 A CN 201910886264A CN 110783537 A CN110783537 A CN 110783537A
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
- H01M4/602—Polymers
- H01M4/606—Polymers containing aromatic main chain polymers
- H01M4/608—Polymers containing aromatic main chain polymers containing heterocyclic rings
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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
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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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- 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 discloses a polypyrrole lithium-sulfur battery material, which comprises a positive electrode and a negative electrode, and is characterized in that the positive electrode comprises a current collector and a positive electrode material, wherein the weight ratio of the current collector to the positive electrode material is 1: 20-30 of active material a and active material b, the composite active material a consisting of polypyrrole and acetylene black and the composite active material b consisting of elemental sulfur and porous carbon are blended, dried and formed, so that the close combination between the composite active material a and the carbon-sulfur composite material can be enhanced, the sulfur and a discharge product are better inhibited from being dissolved in electrolyte, the shuttle effect is prevented, the utilization rate of the sulfur is improved, and the circulation stability and the capacity retention rate of a finished material are improved.
Description
Technical Field
The invention belongs to the field of lithium-sulfur polypyrrole battery materials and particularly relates to a polypyrrole lithium-sulfur battery material.
Background
In recent years, with the decline of oil production and the increase of global environmental pollution, countries around the world generally recognize that the replacement of fuel oil vehicles by clean and pollution-free electric vehicles is a necessary choice for the continuous development of the country. The power battery technology with high specific capacity becomes the key of the development of pure electric vehicles. Meanwhile, the rapid development of communication technology, space technology and national defense industry greatly promotes the demand of rechargeable batteries with small volume and large capacity. At present, lithium ion batteries using lithium cobaltate, lithium manganate, lithium iron phosphate and the like as anode materials are limited by theoretical specific capacity, so that the capacity and energy density are unrealistic to be further improved;
therefore, the development of a high-capacity-density and low-cost lithium ion battery cathode material is particularly critical and urgent, and then, at present, some problems still exist in the lithium-sulfur battery, such as low utilization rate of active materials caused by poor conductivity of elemental sulfur and its reduction product lithium sulfide, low battery capacity retention rate and the like.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings of the prior art and provide a polypyrrole lithium-sulfur battery material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the polypyrrole lithium-sulfur battery material comprises a positive electrode and a negative electrode, wherein the positive electrode comprises a current collector and a positive electrode material, and the weight ratio of the current collector to the positive electrode material is 1: 20-30 of active material a and active material b, wherein the active material a is composed of the following raw materials in parts by weight:
36-40 parts of pyrrole, 0.8-1 part of dibenzoyl peroxide, 43-50 parts of acetylene black, 2-3 parts of triethanolamine, 1-4 parts of stearic acid and 0.01-0.012 part of catalyst.
The catalyst is p-toluenesulfonic acid.
The preparation method of the activated material comprises the following steps:
(1) adding dibenzoyl peroxide into 10-17 times of absolute ethyl alcohol, and uniformly stirring to obtain an initiator solution;
(2) mixing triethanolamine and pyrrole, adding into anhydrous ethanol with the weight 3-4 times of the weight of the mixture, stirring uniformly, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 60-70 ℃, adding the initiator solution, keeping the temperature and stirring for 3-4 hours, discharging, and distilling to remove ethanol to obtain the alcohol amine doped polypyrrole;
(3) heating and melting stearic acid, mixing with acetylene black, adding into deionized water with the weight 10-15 times of that of the mixture, and performing ultrasonic treatment at 55-60 ℃ for 1-2 hours to obtain an acidified filler;
(4) mixing the alcohol amine doped polypyrrole with the acidified filler, uniformly stirring, adding a catalyst, raising the temperature to 90-95 ℃, keeping the temperature and stirring for 1-2 hours, discharging, performing suction filtration, washing a filter cake with water, drying at normal temperature, and performing compression molding to obtain an active material a;
the active material b is formed by mixing elemental sulfur and porous carbon in a weight ratio of 10-13: 1-1.2.
The preparation method of the positive electrode comprises the following steps:
(1) mixing the active material b with a current collector, carrying out heat treatment at the temperature of 600-;
(2) and (3) mixing the active material a with the blank, and drying at 60-80 ℃ for 1-2 hours to obtain the anode.
The negative electrode comprises a current collector, a lithium alloy and a single-walled carbon nanotube, wherein the weight ratio of the current collector to the lithium alloy is 4-5: 1-2.
The lithium alloy is selected from one of lithium hexafluorophosphate, lithium hexafluoroarsenate and lithium perchlorate.
The invention has the advantages that:
the active material takes pyrrole as a monomer, and is polymerized under the action of an initiator by triethanolamine doping to obtain the hydramine doped polypyrrole, then acetylene black is activated by stearic acid, and the polypyrrole and the acetylene black are fully dispersed and compatible by the reaction of the triethanolamine and the stearic acid, so that the conductive stability of the finished material is improved;
according to the invention, the composite active substance a composed of polypyrrole and acetylene black and the composite active substance b composed of elemental sulfur and porous carbon are blended, dried and formed, so that the tight combination between the composite active substance a and the carbon-sulfur composite material can be enhanced, the dissolution of sulfur and a discharge product in an electrolyte can be better inhibited, the shuttle effect is prevented, the utilization rate of sulfur is improved, and the circulation stability and the capacity retention rate of a finished material are improved.
Detailed Description
Example 1
The polypyrrole lithium-sulfur battery material comprises a positive electrode and a negative electrode, wherein the positive electrode comprises a current collector and a positive electrode material, and the weight ratio of the current collector to the positive electrode material is 1: 30, wherein the active material a is composed of the following raw materials in parts by weight:
pyrrole 40, dibenzoyl peroxide 1, acetylene black 50, triethanolamine 3, stearic acid 4, catalyst 0.012.
The catalyst is p-toluenesulfonic acid.
The preparation method of the activated material comprises the following steps:
(1) adding dibenzoyl peroxide into absolute ethyl alcohol with the weight 17 times that of the dibenzoyl peroxide, and uniformly stirring to obtain an initiator solution;
(2) mixing triethanolamine and pyrrole, adding into absolute ethyl alcohol with the weight 4 times of the weight of the mixture, stirring uniformly, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 70 ℃, adding the initiator solution, keeping the temperature and stirring for 4 hours, discharging, and distilling to remove the ethyl alcohol to obtain the alcohol amine doped polypyrrole;
(3) heating and melting stearic acid, mixing with acetylene black, adding into deionized water 15 times of the weight of the mixture, and performing ultrasonic treatment at 60 ℃ for 2 hours to obtain an acidified filler;
(4) mixing the alcohol amine doped polypyrrole with the acidified filler, uniformly stirring, adding a catalyst, raising the temperature to 95 ℃, keeping the temperature and stirring for 2 hours, discharging, performing suction filtration, washing a filter cake with water, drying at normal temperature, and performing compression molding to obtain an active material a;
the active material b is formed by mixing elemental sulfur and porous carbon in a weight ratio of 13: 1.2.
The preparation method of the positive electrode comprises the following steps:
(1) mixing the active material b with a current collector, carrying out heat treatment for 4 hours at 900 ℃ in a protective atmosphere, discharging and cooling to obtain a blank;
(2) and (3) mixing the active material a with the blank, and drying at 80 ℃ for 2 hours to obtain the anode.
The negative electrode comprises a current collector, lithium perchlorate in a weight ratio of 5:2 and a single-walled carbon nanotube.
Example 2
The polypyrrole lithium-sulfur battery material comprises a positive electrode and a negative electrode, wherein the positive electrode comprises a current collector and a positive electrode material, and the weight ratio of the current collector to the positive electrode material is 1: 20, active material a and active material b, wherein the active material a is composed of the following raw materials in parts by weight:
pyrrole 36, dibenzoyl peroxide 0.8, acetylene black 43, triethanolamine 2, stearic acid 1, catalyst 0.01-.
The catalyst is p-toluenesulfonic acid.
The preparation method of the activated material comprises the following steps:
(1) adding dibenzoyl peroxide into 10 times of absolute ethyl alcohol by weight, and uniformly stirring to obtain an initiator solution;
(2) mixing triethanolamine and pyrrole, adding into absolute ethanol with the weight 3 times of the weight of the mixture, stirring uniformly, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 60 ℃, adding the initiator solution, keeping the temperature and stirring for 3 hours, discharging, and distilling to remove ethanol to obtain the alcohol amine doped polypyrrole;
(3) heating and melting stearic acid, mixing with acetylene black, adding into deionized water with the weight being 10 times of that of the mixture, and carrying out ultrasonic treatment at 55 ℃ for 1 hour to obtain an acidified filler;
(4) mixing the alcohol amine doped polypyrrole with the acidified filler, uniformly stirring, adding a catalyst, raising the temperature to 90 ℃, keeping the temperature and stirring for 1 hour, discharging, performing suction filtration, washing a filter cake with water, drying at normal temperature, and performing compression molding to obtain an active material a;
the active material b is formed by mixing elemental sulfur and porous carbon in a weight ratio of 10: 1.
The preparation method of the positive electrode comprises the following steps:
(1) mixing the active material b with a current collector, carrying out heat treatment at 600 ℃ for 3 hours in a protective atmosphere, discharging and cooling to obtain a blank;
(2) and (3) mixing the active material a with the blank, and drying at 60 ℃ for 1 hour to obtain the anode.
The negative electrode comprises a current collector, lithium hexafluorophosphate and a single-walled carbon nanotube in a weight ratio of 4: 1.
And (3) performance testing:
the detection method comprises the following steps: the polypyrrole lithium sulfur batteries of example 1 and example 2 and the commercial lithium sulfur battery were charged at a constant current of 0.2C at room temperature, with an upper limit voltage of 2.8V; discharging at a constant current of 0.2C, with a lower limit voltage of 1.5V, taking one charge-discharge process as a cycle, recording the first discharge specific capacity, measuring the specific capacity of the battery after 150 cycles, and calculating the capacity retention rate, wherein the specific capacity is calculated based on the sulfur capacity of an active material in the anode;
polypyrrole lithium sulfur battery of example 1 of the invention:
the first discharge specific capacity is as follows: 1134.3 mAh/g;
the specific capacity of the battery after 150 cycles is determined: 1041 mAh/g;
capacity retention ratio: 91.77 percent.
Polypyrrole lithium sulfur battery of embodiment 2 of the invention:
the first discharge specific capacity is as follows: 1121.9 mAh/g;
the specific capacity of the battery after 150 cycles is determined: 1028.4 mAh/g; capacity retention ratio: 91.67 percent.
Commercial lithium sulfur batteries:
the first discharge specific capacity is as follows: 1115.3 mAh/g;
the specific capacity of the battery after 150 cycles is determined: 665.4 mAh/g; capacity retention ratio: 59.67 percent.
Claims (6)
1. The polypyrrole lithium-sulfur battery material comprises a positive electrode and a negative electrode, and is characterized in that the positive electrode comprises a current collector and a positive electrode material, wherein the weight ratio of the current collector to the positive electrode material is 1: 20-30 of active material a and active material b, wherein the active material a is composed of the following raw materials in parts by weight:
36-40 parts of pyrrole, 0.8-1 part of dibenzoyl peroxide, 43-50 parts of acetylene black, 2-3 parts of triethanolamine, 1-4 parts of stearic acid and 0.01-0.012 part of catalyst.
2. The lithium polypyrrole sulfur battery material according to claim 1, wherein the catalyst is p-methyl benzene sulfonic acid.
3. The lithium polypyrrole sulfur battery material according to claim 1, wherein the preparation method of the activation material comprises the following steps:
(1) adding dibenzoyl peroxide into 10-17 times of absolute ethyl alcohol, and uniformly stirring to obtain an initiator solution;
(2) mixing triethanolamine and pyrrole, adding into anhydrous ethanol with the weight 3-4 times of the weight of the mixture, stirring uniformly, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 60-70 ℃, adding the initiator solution, keeping the temperature and stirring for 3-4 hours, discharging, and distilling to remove ethanol to obtain the alcohol amine doped polypyrrole;
(3) heating and melting stearic acid, mixing with acetylene black, adding into deionized water with the weight 10-15 times of that of the mixture, and performing ultrasonic treatment at 55-60 ℃ for 1-2 hours to obtain an acidified filler;
(4) mixing the alcohol amine doped polypyrrole with the acidified filler, uniformly stirring, adding a catalyst, raising the temperature to 90-95 ℃, keeping the temperature and stirring for 1-2 hours, discharging, performing suction filtration, washing a filter cake with water, drying at normal temperature, and performing compression molding to obtain an active material a;
the active material b is formed by mixing elemental sulfur and porous carbon in a weight ratio of 10-13: 1-1.2.
4. The lithium polypyrrole sulfur battery material according to claim 1, wherein the preparation method of the positive electrode is as follows:
(1) mixing the active material b with a current collector, carrying out heat treatment at the temperature of 600-;
(2) and (3) mixing the active material a with the blank, and drying at 60-80 ℃ for 1-2 hours to obtain the anode.
5. The lithium polypyrrole sulfur battery material according to claim 1, wherein the negative electrode comprises a current collector and a lithium alloy, single-walled carbon nanotube with a weight ratio of 4-5: 1-2.
6. The lithium polypyrrole sulfur battery material according to claim 5, wherein the lithium alloy is selected from one of lithium hexafluorophosphate, lithium hexafluoroarsenate and lithium perchlorate.
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