CN109286027B - Lithium nitrogen oxygen battery with Fe nano-particles and carbon composite material as anode catalyst - Google Patents
Lithium nitrogen oxygen battery with Fe nano-particles and carbon composite material as anode catalyst Download PDFInfo
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- CN109286027B CN109286027B CN201811084277.1A CN201811084277A CN109286027B CN 109286027 B CN109286027 B CN 109286027B CN 201811084277 A CN201811084277 A CN 201811084277A CN 109286027 B CN109286027 B CN 109286027B
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9041—Metals 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
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/08—Hybrid cells; Manufacture thereof composed of a half-cell of a fuel-cell type and a half-cell of the secondary-cell type
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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
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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- 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 relates to a lithium nitrogen oxygen battery taking a Fe nano-particle and Ketjen black composite material as a positive electrode catalyst, wherein the catalyst is a composite material in which metal iron nano-particles are highly dispersed on nano-carbon. The invention adopts environment-friendly nontoxic reagents, and the synthesized composite material can be used as a catalyst for preparing the anode of the lithium nitrogen oxygen battery, and the method comprises the following steps: the catalyst, the binder and the solvent are uniformly mixed, the mixture is uniformly coated on conductive carbon paper, and the positive electrode of the battery is obtained after drying. The invention has the advantages that: the catalyst can improve the electrocatalytic performance of the battery, simultaneously, the battery has good circulation stability, and the battery assembled by the material also has higher specific energy in the air; the catalyst is simple in preparation process, low in cost and easy to obtain, is environment-friendly, has a great auxiliary effect on improving the performance of the lithium nitrogen oxygen battery, and has the potential of being widely applied.
Description
Technical Field
The invention relates to a lithium nitrogen oxygen battery taking Fe nano-particles and carbon composite materials as a positive electrode catalyst.
Background
The lithium air battery has the advantages of high specific energy, no pollution, stable discharge platform and the like, so the lithium air battery has high potential to be applied to actual life. With the rapid development of the modern society, people have higher and higher requirements on a battery system with high energy storage. The lithium-air battery has the highest specific energy, and plays a great role if applied to the fields of electronic equipment, communication devices and the like. However, the lithium-air battery at the present stage still has many technical problems to be solved urgently, such as low charging and discharging efficiency, too high charging overvoltage, and the disadvantage of using pure oxygen as the working atmosphere, but the cost of the lithium-air battery is greatly increased and the application range of the lithium-air battery is greatly limited by using pure oxygen as the working atmosphere. It is known that air contains 78% nitrogen and only about one fifth of oxygen, and therefore the electrochemical reaction of an air cell in this atmosphere is certainly different from that of pure oxygen. At normal temperature, the lithium metal reacts with nitrogen in the air to form lithium nitride. In the early 90 s of the last century, electrolytes containing lithium perchlorate were used in the electrocatalytic reduction of nitrogen to ammonia (Chemistry Letters 1993, 22, 851-. Pure nitrogen applications have also been successfully demonstrated in lithium air battery systems (Chem 2017, 2, 525-. These studies all show that nitrogen can also participate in the reaction in the battery system and that the energy given by nitrogen is not negligible. Therefore, a nitrogen-oxygen mixed gas system is introduced into a lithium gas battery system, and the aim is to research electrochemical reaction in the mixed system, optimize various reaction conditions, improve electrochemical performance and specific discharge energy and finally truly realize the lithium air battery running in air. Similar to the existing lithium oxygen battery, the lithium nitrogen oxygen has the problems of low charge and discharge efficiency and over-high charge overvoltage, so that an efficient anode catalyst is needed to accelerate the decomposition of discharge products, improve the charge efficiency and reduce the charge voltage. The material compounded by the transition metal and the carbon substrate has high catalytic performance, is simple and easy to obtain, has low price and is environment-friendly. Also, transition metal and carbon-based composite materials are widely used in lithium oxygen batteries and lithium carbon dioxide batteries (chem. Commun 2014, 50, 776 and Advanced Science 2017, 1700567). The materials can obviously reduce the charging voltage and improve the cycling stability of the battery. However, in the lithium nitrogen oxygen battery system, there is no study on the positive electrode catalyst.
Chinese patent CN103560256A discloses a lithium-air battery anode containing a novel catalyst and a preparation method thereof, wherein metal nanoparticles are highly dispersed on a carbon nanosheet to form a metal/carbon composite material, and the metal/carbon composite material is used as a catalyst of the lithium-air battery anode to improve the catalytic activity of the anode and improve the cycle stability of the lithium-air battery. The metal nanoparticles are cobalt, nickel, copper, zinc, manganese, chromium, molybdenum, vanadium or yttrium. The invention provides a lithium nitrogen oxygen battery anode with Fe/Kb as a catalyst, which is characterized in that a lithium air battery system which can enable a battery to operate in nitrogen and oxygen mixture and has a high-efficiency catalytic action, namely Fe/Kb (Keqin black), is provided, the cycle stability of the battery is improved, and the battery can actually operate in the air.
Disclosure of Invention
The invention aims to provide a lithium nitrogen oxygen battery taking Fe nano-particles and carbon composite materials as a positive electrode catalyst. The Fe nano-particles and carbon composite material is a positive electrode material with efficient catalytic action, and the Fe metal nano-particles are formed by highly dispersing the Fe metal nano-particles on Ketjen black or carbon nano-tubes through hydrothermal reaction and are used as a catalyst of a battery positive electrode, so that the catalytic activity of the positive electrode is improved, the battery running in a nitrogen-oxygen mixed system is realized, and the high discharge specific energy and the cycling stability are achieved.
The lithium nitrogen oxygen battery taking the Fe nano-particles and the carbon composite material as the anode catalyst comprises an anode, a lithium cathode, a diaphragm, electrolyte, a current collector and a battery shell; the anode material is prepared from a catalyst, a carbon material, a binder and a dispersion solution, wherein the mass ratio of the catalyst to the electrode is 70-90%, and the mass ratio of the binder to the electrode is 10-30%.
The binder is one or a mixture of more than two of Polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), sodium carboxymethyl cellulose (CMC), polyethylene glycol (PVA) and styrene-butadiene resin (SBR) in any proportion.
The electrolyte is one of bis (trifluoromethyl) sulfonyl imide lithium, bis (fluoro) sulfonyl imide lithium, lithium trifluoromethanesulfonate, lithium trifluoroacetate, lithium nitrate and lithium perchlorate dissolved in ethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, dimethyl sulfoxide and 1-butyl-1 methyl-pyrrole bis (trifluoromethyl sulfonyl) imide.
The dispersion solution is N-methyl pyrrolidone (NMP). The battery diaphragm is one of glass fiber or polytetrafluoroethylene.
The electrode is as follows: fe nanoparticles and carbon composite materials, Fe nanoparticles and Keqin black composite materials or Fe nanoparticles and carbon nanotube composite materials.
The Fe nano-particle and Ketjen black (Kb) or carbon nano tube composite material is prepared by taking soluble ferric nitrate and Ketjen black or carbon nano tubes as raw materials and performing hydrothermal reaction, specifically, ferric nitrate, Ketjen black or carbon nano tubes, urea and ethylene glycol are subjected to ultrasonic mixing, poured into a reaction kettle and subjected to high-temperature hydrothermal reaction for 4 hours, a product is washed by ethanol and then dried, pre-sintered in a tube furnace, and then calcined at high temperature. Wherein the mass ratio of the Ketjen black or the carbon nano tube to the ferric nitrate, the urea and the ethylene glycol is 1: 8:16: 780.
The grain diameter of the Fe nano-particles is 60-200 nm.
The preparation method of the positive electrode catalyst Fe nano-particles and Ketjen black (Kb) or carbon nano-tube composite material of the lithium nitrogen oxygen battery comprises the following steps:
uniformly stirring Ketjen black or carbon nano tubes with ferric nitrate, urea and ethylene glycol respectively at room temperature for 3-6 h, performing ultrasonic treatment for 1 h, pouring into a reaction kettle, and keeping in an oven at 200 ℃ for 4h at 150-; washing with ethanol until the supernatant is clear, taking out the sample, and drying in an oven at 80 ℃ for 24 h; presintering for 3 h at the temperature of 300-350 ℃ in an argon environment, calcining for 6-8 h at the temperature of 750-800 ℃, and taking out from the tube furnace.
The preparation method of the positive electrode of the lithium nitrogen oxygen battery provided by the invention comprises the following steps:
1) adding the Fe nano particles, the Ketjen black (Kb) or the carbon nano tube composite material and the binder into a N-methyl pyrrolidone (NMP) solvent according to the weight, uniformly mixing, and performing ultrasonic treatment for 30 minutes to obtain the slurry of the positive electrode catalyst.
2) And (3) dropwise adding the mixture onto conductive carbon paper, and drying to obtain the positive pole piece.
The carbon material also comprises one or a mixture of more than two of acetylene black, superconducting carbon black, carbon fiber and graphene in any proportion.
The invention has the advantages that: the composite material of the metal nanoparticles and the carbon with good conductivity is applied to the anode of the lithium nitrogen oxygen battery, the anode shows higher specific capacity and excellent cycling stability, the specific capacity reaches 3888 mAh/g under the current density of 100 mA/g, and the air battery using the material as the air anode can stably cycle for 48 circles in the air atmosphere, so that the assembled button battery can simultaneously light 19 light-emitting diodes in the air and keep the lighting time for 18 hours. The excellent electrochemical performance is mainly because the metallic iron nano particles are uniformly dispersed on the Ketjen black carrier, so that abundant active sites are provided for electrochemical reaction, and the metallic iron nano particles have good conductivity, so that the battery assembled by the material has high specific capacity. And the Fe/Kb preparation process is simple, and the raw materials are cheap and easy to obtain, so that the composite material of the metal nano particles and the carbon material has wide application prospect in the field of lithium nitrogen oxygen batteries.
Drawings
FIG. 1 is an XRD pattern of Fe/Kb composite material.
FIG. 2 is an SEM image of an Fe/Kb composite.
FIG. 3 is a TEM image of the Fe/Kb composite.
FIG. 4 is a graph showing the cycle performance of a lithium nitrogen oxygen battery using an Fe/Kb composite material as a catalyst.
FIG. 5 shows the cycling performance of a lithium-air positive electrode with Fe/Kb composite as a catalyst in air.
FIG. 6 is a graph showing the performance of a lithium air anode with Fe/Kb composite as a catalyst for lighting a light emitting diode in air.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1:
a lithium nitrogen oxygen battery taking Fe/Kb as a catalyst comprises iron nanoparticles highly dispersed on Ketjen black (EC-600 JD Japan lion king), and the material is synthesized by a hydrothermal method and comprises the following steps: 50mg of Keqin black, 0.4g of ferric nitrate, 0.819g of urea and 35mL of ethylene glycol are uniformly stirred for 3 hours at room temperature, subjected to ultrasonic treatment for 1 hour, poured into a reaction kettle and kept in an oven at 200 ℃ for 4 hours; washing with ethanol until the supernatant is clear, taking out the sample, and drying in an oven at 80 ℃ for 24 h; presintering for 3h at 350 ℃ in an argon environment, calcining for 8h at 750 ℃, and taking out from a tubular furnace to obtain the Fe/Kb composite catalyst. The resulting composite was characterized as shown in FIGS. 1-3.
The preparation method of the anode plate by using the catalyst comprises the following steps: 1) dissolving a Fe/Kb composite material and polyvinylidene fluoride (PVDF) in N-methyl pyrrolidone (NMP) according to the mass percentage of 9:1, and uniformly mixing the materials to obtain a liquid mixture; 2) and (3) coating the liquid mixture on the conductive carbon paper. Placing the electrode sheet at 80oAnd C, drying in an oven for 12h, and assembling into a simulated battery. The lithium sheet is a counter electrode and a reference electrode. The electrochemical performance of the cell is characterized in figures 4-6.
FIG. 1 is an XRD pattern of an Fe/Kb composite. Analysis shows that the composite material contains carbon and metallic iron, and the metallic nano-particles belong to a cubic system.
FIG. 2 is a scanning electron micrograph of the Fe/Kb composite. It can be seen from the figure that: the material successfully composites iron nanoparticles on ketjen black.
FIG. 3 is a transmission electron micrograph of the Fe/Kb composite. It can be seen from the figure that: the iron nano-particles with the particle size of 10-100 nm are uniformly distributed on the Ketjen black, so that the active sites of the electrochemical reaction are greatly increased, and the catalytic performance of the material is enhanced.
FIG. 4 is a graph showing the cycle performance of a lithium nitrogen oxygen battery using an Fe/Kb composite material as a positive electrode. The test conditions were: the current is 100 mA/g, and the voltage range is 2-4.5V. The results show that: the first-cycle capacity of the battery can reach 3888 mA h/g by taking Fe/Kb as the anode, which shows that the Fe/Kb catalyst has excellent electrochemical catalytic performance.
In FIG. 5, the battery using the Fe/Kb composite material as the anode can stably circulate for 48 circles in the air, and the discharge plateau is about 2.75V, so that the battery has relatively stable cycle performance.
FIG. 6 is a graph showing the performance of an air battery using a lithium air positive electrode with Fe/Kb composite as a catalyst in air. The battery can light 19 LED lamps at a time in air and hold for 18 hours. The lithium air battery has very high specific energy, can stably output energy in air, and is a lithium air battery model with practical application potential.
Example 2:
a novel catalyst material applied to a lithium nitrogen oxygen battery comprises iron nanoparticles (Fe/CNTs) highly dispersed on carbon nanotubes, and the material is synthesized by a hydrothermal method, and comprises the following steps: dissolving 0.2 g of ferric nitrate, 0.4g of urea and 25 mg of carbon nano tube (XFM 40 Nanjing pioneer nano) in 35 ml of ethylene glycol, stirring for 3 hours at room temperature, and performing ultrasonic treatment for 1 hour; pouring into a reaction kettle, and keeping for 4 hours in a baking oven at 200 ℃; washing with ethanol, clarifying the supernatant, taking out a sample, drying in an oven at 80 ℃ for 24h, presintering at 350 ℃ for 3h under the argon environment, calcining at 750 ℃ for 8h, and taking out from a tube furnace to obtain the Fe/CNTs composite catalyst.
The preparation method of the anode plate by using the catalyst comprises the following steps: 1) dissolving Fe/CNTs and PVDF in Nitrogen Methyl Pyrrolidone (NMP) according to the mass percentage of 90:10, and uniformly mixing the materials to obtain a liquid mixture; 2) and (3) coating the liquid mixture on conductive carbon paper to prepare the positive pole piece. Placing the electrode sheet at 80oAnd C, drying for 12 h in an oven, and assembling into a simulated battery.
Claims (3)
1. An application of a Fe nano-particle and Ketjen black or carbon nano-tube composite material as a positive electrode catalyst in a lithium nitrogen oxygen battery is disclosed, wherein the preparation method of the composite material comprises the following steps:
uniformly stirring Ketjen black or carbon nano tubes with ferric nitrate, urea and ethylene glycol respectively at room temperature for 3-6 h, performing ultrasonic treatment for 1 h, pouring into a reaction kettle, and keeping in an oven at 200 ℃ for 4h at 150-; washing with ethanol until the supernatant is clear, taking out the sample, and drying in an oven at 80 ℃ for 24 h; presintering for 3 h at the temperature of 300-350 ℃ in an argon environment, calcining for 6-8h at the temperature of 750-800 ℃, and taking out from the tube furnace;
the mass ratio of the Ketjen black or the carbon nano tube to the ferric nitrate, the urea and the ethylene glycol is 1: 8:16: 780.
2. The use according to claim 1, wherein the Fe nanoparticles have a particle size of 60-200 nm.
3. The use according to claim 1, characterized in that the method for preparing the positive electrode of a lithium nitrogen oxygen cell comprises the following steps:
1) adding a catalyst Fe nano particle and a Ketjen black (Kb) composite material or a Fe nano particle and carbon nano tube composite material and a binder into a N-methyl pyrrolidone (NMP) solvent according to the measurement, uniformly mixing, and performing ultrasonic treatment for 30 minutes to obtain slurry of the positive catalyst;
2) dropwise adding the mixture onto conductive carbon paper, and drying to obtain a positive pole piece;
the weight ratio of the Fe nano-particles and Keqin black (Kb) composite material or the Fe nano-particles and carbon nano-tube composite material in the catalyst to the electrode is 70-90%; the mass ratio of the binder to the electrode is 10-30%.
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| WO2003032419A2 (en) * | 2001-10-09 | 2003-04-17 | Metalic Power, Inc. | Methods of producing oxygen reduction catalyst |
| CN1713425A (en) * | 2004-06-14 | 2005-12-28 | 中国科学院大连化学物理研究所 | Electrode of fuel battery with proton exchange membrane and its production |
| CN1776947A (en) * | 2004-11-16 | 2006-05-24 | 三星Sdi株式会社 | Metal catalyst and fuel cell with electrode including the same |
| CN103560256A (en) * | 2013-10-28 | 2014-02-05 | 南开大学 | Positive electrode of lithium air battery and preparation method of positive electrode |
| CN104415758A (en) * | 2013-09-06 | 2015-03-18 | 中国科学院大连化学物理研究所 | Preparation method and applications of non-noble metal electrocatalyst |
| CN106410174A (en) * | 2016-10-25 | 2017-02-15 | 中国科学院长春应用化学研究所 | Electrodes of lithium-nitrogen secondary battery and lithium-nitrogen secondary battery |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003032419A2 (en) * | 2001-10-09 | 2003-04-17 | Metalic Power, Inc. | Methods of producing oxygen reduction catalyst |
| CN1713425A (en) * | 2004-06-14 | 2005-12-28 | 中国科学院大连化学物理研究所 | Electrode of fuel battery with proton exchange membrane and its production |
| CN1776947A (en) * | 2004-11-16 | 2006-05-24 | 三星Sdi株式会社 | Metal catalyst and fuel cell with electrode including the same |
| CN104415758A (en) * | 2013-09-06 | 2015-03-18 | 中国科学院大连化学物理研究所 | Preparation method and applications of non-noble metal electrocatalyst |
| CN103560256A (en) * | 2013-10-28 | 2014-02-05 | 南开大学 | Positive electrode of lithium air battery and preparation method of positive electrode |
| CN106410174A (en) * | 2016-10-25 | 2017-02-15 | 中国科学院长春应用化学研究所 | Electrodes of lithium-nitrogen secondary battery and lithium-nitrogen secondary battery |
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