CN111668536A - Preparation method of metal aluminum-cyano organic matter secondary battery - Google Patents
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- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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Abstract
A preparation method of a metal aluminum-cyano organic matter secondary battery belongs to the field of electrochemical batteries. Comprises a cyano (-C [ identical to ] N) organic positive electrode, an aluminum/aluminum alloy negative electrode, an aluminum chloride and inorganic acid salt electrolyte and optionally a separator. The organic positive electrode material takes cyano group as electrochemical oxidation-reduction active site, and during discharge, positive organic substance is reduced into electronegative cyano organic molecule, and positive aluminum complex ion (such as AlCl) dissociated from electrolyte2 +) When the bond is charged, the two are reversibly dissociated, and the electronegative cyano-group organic molecule is reoxidized into an electrically neutral cyano-group organic molecule. The discharging and charging voltage ranges of the metal aluminum-cyano organic matter battery are 0.8-2.0V and 1.0-2.2V respectively. The cyano organic anode adopted by the invention has the advantages of high output voltage and high specific capacity,and the molecules can be designed, and are cheap and easy to obtain. The metal aluminum secondary battery based on the organic anode has higher energy density and rate capability, and is expected to become a next-generation advanced energy storage secondary battery with high performance and low cost.
Description
Technical Field
The invention relates to a metal aluminum-cyano organic matter secondary battery, belonging to the field of electrochemical batteries. Particularly provides a cyano-group organic anode which is low in price, simple and easily available and environment-friendly, and finally obtains a metal aluminum-cyano-group organic matter secondary battery with high energy density and long cycle stability.
Background
In recent years, with the continuous decrease of coal, oil and natural gas and the environmental pressure caused by the use of the same, the development and utilization of clean renewable energy sources have become hot spots of current research. In consideration of the characteristics of the renewable energy source such as volatility, intermittency and periodicity, the storage of electric energy is very critical. Rechargeable metallic aluminum secondary batteries are considered to be ideal carriers for large-scale energy storage due to abundant aluminum resources, low price and high safety. Metal aluminum secondary batteries with high energy density and excellent stability have become hot spots in the field of energy storage. The positive electrode material is the key to determine the performance of the metal aluminum battery. Currently, the anode materials of metal aluminum batteries widely studied are mainly inorganic materials such as graphite and metal-based compounds (CuS, CoS, Ni)2S, CuP). However, the graphite positive electrode has a low capacity, slow ion intercalation/deintercalation kinetics, large volume expansion, structural damage, and a low battery capacity. The discharge voltage of the anode of the metal compound is low, and the anode is particularly easy to dissolve and corrode in the ionic liquid electrolyte and poor in cycle stability.
Compared with inorganic materials, organic materials have the advantages of abundant resources, designable structure and the like. More importantly, the organic material has weak intermolecular interaction, and the volume and structure of the material are not obviously changed in the charge-discharge process, so that the method is beneficial to prolonging the cycle service life of the battery. Therefore, the organic matter is a positive electrode material of the metal aluminum secondary battery with application potential. So far, metal aluminum secondary batteries using organic substances as the positive electrode are relatively few, and researchers have found that only carbonyl group (-C ═ O) containing organic substances can be used as the positive electrode material of metal aluminum batteries, but the actual capacity is low (Nature Energy,2019,4(1): 51-59). Therefore, the design and development of novel organic cathode materials to construct high-performance metal aluminum-organic secondary batteries have very important practical significance and application potential.
Disclosure of Invention
Aiming at the research background, the invention provides a metal aluminum-cyano organic matter secondary battery, which takes cyano (-C ≡ N) containing organic matter as a positive electrode material, a cyano group as an electrochemical redox active site, and during discharge, reduced electronegative cyano organic molecules and electropositive aluminum complex ions (AlCl) dissociated from electrolyte2 +、AlCl2+Or Al3+) When the bond is charged, the two are reversibly dissociated, and the electronegative cyano-group organic molecule is reoxidized into an electrically neutral cyano-group organic molecule. The metal aluminum-cyano organic secondary battery has high specific capacity and discharge voltage, and can improve the energy density of the metal aluminum battery. In order to achieve the purpose, the invention provides the following technical scheme:
a metal aluminum-cyano organic matter secondary battery is characterized in that cyano (-C [ identical to ] N) organic matter is used as a positive electrode material, metal aluminum or aluminum alloy is used as a negative electrode, and aluminum chloride-inorganic acid salt is used as electrolyte. The number of cyano groups in the organic substance is 1-6. The cyano-group organic matter, the conductive additive and the adhesive are uniformly dispersed in the solvent, coated on a conductive current collector, dried at 60-100 ℃ and under the vacuum pressure of 1-100 Pa to prepare a positive electrode film, separated from a negative electrode by a diaphragm, injected with the electrolyte, and assembled to obtain the metal aluminum-cyano-group organic matter secondary battery. During discharge, the positive organic matter is reduced into electronegative cyano organic molecules, and the electronegative cyano organic molecules and the electropositive aluminum complex ions (AlCl) dissociated from the electrolyte2 +、AlCl2+Or Al3+) And bonding, wherein during charging, electronegative cyano organic molecules are dissociated from electropositive aluminum complex ions and are reoxidized into electroneutral organic matters. The discharging and charging voltage ranges of the metal aluminum-cyano organic matter battery are 0.8-2.0V and 1.0-2.2V respectively, and the charging and discharging current density ranges are 0.01-10A g-1Specific capacity of 50-300mAh g-1。
Further, the organic positive electrode containing a cyano group is one or more of benzonitrile, cinnamonitrile, 4-pyridylacetonitrile, diphenylacetonitrile, 4-cyanobiphenyl, 1-naphthonitrile, 2-naphthonitrile, 10, 11-dihydro-5H-dibenzo [ A, D ] cycloheptene-5-carbonitrile, and 6-cyanoquinoline; the positive electrode of the organic matter containing two cyano groups is one or more than two of 1, 4-benzenediacetonitrile, phthalonitrile, 2-cyanophenylacetonitrile naphthalene-1, 4-dinitrile, 9, 10-dicyanoanthracene and m-phthalonitrile; the organic positive electrode containing three cyano groups is one or more than two of (benzene-1, 3, 5-triacyl) acetonitrile, 1,3, 5-tri (4-cyanophenyl) benzene, [1,3, 5-tri (4-cyanoethyl benzene) benzene and 2,4, 6-tricyano-1, 3, 5-trimethylbenzene; the organic positive electrode containing four cyano groups is one or more than two of 5,10,15, 20-tetra (4-cyanophenyl) porphyrin, 7,8, 8-tetracyano-p-quinodimethane, tetra (4-cyanophenyl) methane, tetracyanoethylene and 1,2,4, 5-benzene tetracyanonitrile; the organic positive electrode containing six cyano groups is hexacyanohexatriphenylene.
Further, the negative electrode is binary or multi-element alloy formed by simple substance aluminum or aluminum and metal copper, iron, nickel, lead, bismuth, tin and silver.
Further, the mass ratio of the cyano-group organic matter to the conductive additive to the binder is (6-8): (3-1): 1.
Further, the conductive additive is one or more of acetylene black, graphite powder, carbon nanotubes and graphene.
Further, the conductive current collector is one of a tantalum sheet, a tantalum mesh and carbon cloth.
Further, the aluminum chloride-inorganic acid salt electrolyte is one of aluminum chloride-triethylamine hydrochloride, aluminum chloride-1-butyl-3-methylimidazole chloride and aluminum chloride-phenyltrimethylammonium chloride, and the molar ratio of aluminum chloride to inorganic acid salt in the electrolyte is 1: 1-3: 1.
Further, the solvent is one or a mixture of more than two of N-methyl pyrrolidone, N-dimethylformamide, N-dimethylacetamide and dimethyl sulfoxide in any proportion
According to the invention, through adjusting the number of cyano groups and the occurrence molecular structure in the organic matter, the mass ratio of the cyano groups is improved, the electron transfer number can be increased, the specific capacity is improved, and meanwhile, high discharge voltage is displayed, so that the energy density of the battery is improved. In general, compared with the prior art, the technical scheme of the invention can obtain the following beneficial effects:
(1) the molecular structure of the organic anode and the number of cyano groups can be flexibly designed, the number of active sites is large, energy storage and release are realized based on reversible bonding-dissociation of the cyano groups and electropositive aluminum complex ions, a plurality of aluminum complex ions can be bonded, and the specific capacity of the battery is high;
(2) the positive electrode does not have an embedding-stripping process, so that the structural damage of the positive electrode is avoided, and the improvement of the cycling stability of the battery is facilitated;
(3) the synthetic raw materials of the organic matter are low in price and wide in source, the preparation process is green and environment-friendly, and the cost of the battery can be reduced.
Drawings
Fig. 1 is a schematic diagram of the battery structure of example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
The button cell is assembled by fully and uniformly mixing 48mg of hexacyanohexatriphenylene, 6mg of acetylene black and 6mg of polyvinylidene fluoride in N, N-dimethylformamide, coating the mixture on a tantalum sheet, and performing vacuum drying for 24 hours at 60 ℃ under the vacuum pressure of 1Pa to prepare a positive electrode membrane, wherein the prepared electrode membrane is used as a positive electrode, glass fiber is used as a diaphragm, aluminum chloride-triethylamine hydrochloride ionic liquid with the molar ratio of 1.2 is used as electrolyte, and metal aluminum is used as a negative electrode. Assembled cell at 1000mA g-1Constant current charging and discharging are carried out at the current density of (3).
Example 2
Mixing 24mg of benzonitrile, 24mg of graphite powder and 6mg of polyvinylidene fluoride in N-methylpyrrolidone, uniformly coating the mixture on a tantalum mesh, coating the tantalum mesh, and drying the mixture in vacuum at 80 ℃ and under the vacuum pressure of 50Pa for 8 hours to prepare a positive electrode membrane, wherein the prepared electrode membrane is used as a positive electrode, and glass is used as the positive electrodeThe fiber is a diaphragm, the aluminum chloride-1-butyl-3-methylimidazole chloride ionic liquid with the molar ratio of 1.6 is used as electrolyte, and the metal aluminum is used as a negative electrode to assemble the soft package battery. The assembled battery was at 100mA g-1Constant current charging and discharging are carried out at the current density of (3).
Example 3
The method comprises the steps of fully and uniformly mixing 36mg of tetracyanoquinodimethane, 18mg of acetylene black and 6mg of polyvinylidene fluoride in N-methyl pyrrolidone, coating the mixture on a tantalum foil, and performing vacuum drying at 60 ℃ under the vacuum pressure of 5Pa for 12 hours to prepare a positive electrode film, wherein the prepared electrode film is used as a positive electrode, glass fiber is used as a diaphragm, aluminum chloride-1-butyl-3-methylimidazole chloride ionic liquid with the molar ratio of 1.3 is used as electrolyte, and metal aluminum is used as a negative electrode to assemble the soft package battery. The assembled cell was operated at 500mA g-1Constant current charging and discharging are carried out at the current density of (3).
Example 4
Fully and uniformly mixing 30mg of 2-cyanobenzene acetonitrile naphthalene-1, 4-dinitrile, 6mg of acetylene black and 6mg of polyvinylidene fluoride in N, N-dimethylformamide, coating the mixture on a tantalum foil, and performing vacuum drying for 12 hours at 100 ℃ under the vacuum pressure of 10Pa to prepare a positive electrode film, wherein the prepared electrode film is used as a positive electrode, glass fiber is used as a diaphragm, aluminum chloride-phenyltrimethylammonium chloride with the molar ratio of 2 is used as electrolyte, and metal aluminum is used as a negative electrode to assemble the soft package battery. The assembled cell was at 2000mA g-1Constant current charging and discharging are carried out at the current density of (3).
Example 5
The button cell is assembled by fully and uniformly mixing 48mg of m-phthalonitrile, 6mg of carbon nano tube and 6mg of polyvinylidene fluoride in N, N-dimethylformamide, coating the mixture on a tantalum mesh, and performing vacuum drying for 12 hours at the temperature of 60 ℃ and under the vacuum pressure of 50Pa to prepare a positive electrode membrane, wherein the prepared electrode membrane is used as a positive electrode, glass fiber is used as a diaphragm, aluminum chloride-1-butyl-3-methylimidazole chloride ionic liquid with the molar ratio of 2.5 is used as electrolyte, and metal aluminum is used as a negative electrode. The assembled battery is at 5000mA g-1Constant current charging and discharging are carried out at the current density of (3).
Example 6
42mg of 1,3, 5-tris (4-cyanophenyl) benzene, 3mg of carbon nanotubes, 3mg of graphite powder and 6mg of polyvinylidene fluorideThe button cell is assembled by fully and uniformly mixing dimethyl sulfoxide, coating the mixture on a tantalum mesh, and performing vacuum drying for 12 hours at 80 ℃ and under the vacuum pressure of 70Pa to prepare a positive electrode membrane, wherein the prepared electrode membrane is taken as a positive electrode, glass fiber is taken as a diaphragm, the glass fiber is taken as the diaphragm, aluminum chloride-1-butyl-3-methylimidazole chloride ionic liquid with the molar ratio of 2.5 is taken as electrolyte, and metal aluminum is taken as a negative electrode. The assembled battery is at 10A g-1Constant current charging and discharging are carried out at the current density of (3).
Example 7
The method comprises the steps of fully and uniformly mixing 36mg of 9, 10-dicyanoanthracene, 6mg of graphene and 6mg of polyvinylidene fluoride in N, N-dimethylacetamide, coating the mixture on a tantalum mesh, and performing vacuum drying for 12 hours at 90 ℃ under the vacuum pressure of 30Pa to prepare a positive electrode membrane, wherein the prepared electrode membrane is used as a positive electrode, glass fiber is used as a diaphragm, aluminum chloride-1-butyl-3-methylimidazole chloride ionic liquid with the molar ratio of 2.5 is used as electrolyte, and metal aluminum is used as a negative electrode to assemble the soft package battery. The assembled battery was operated at 800mA g-1Constant current charging and discharging are carried out at the current density of (3).
It should be noted that, according to the above embodiments of the present invention, those skilled in the art can fully implement the full scope of the present invention as defined by the independent claims and the dependent claims, and implement the processes and methods as the above embodiments; and the invention has not been described in detail so as not to obscure the present invention.
The above description is only a part of the embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (8)
1. A preparation method of a metal aluminum-cyano organic matter secondary battery is characterized in that a cyano (-C [ identical to ] N) organic matter is used as a positive electrode material, metal aluminum or aluminum alloy is used as a negative electrode, and aluminum chloride-inorganic acid salt is used as electrolyte; the number of cyano groups in the cyano organic matter is 1-6; the cyano organic matter, the conductive additive and the adhesive are uniformly dispersed in the solvent, and are coated on the conductive current collector at the temperature of 60-100 ℃ and the vacuum pressure of 1 Pa-100Drying under Pa to prepare a positive electrode film, separating the positive electrode film from a negative electrode film by a diaphragm, injecting electrolyte, and assembling to obtain the metal aluminum-cyano organic matter secondary battery; during discharging, the positive organic matter is reduced into electronegative cyano organic molecules and is bonded with electropositive aluminum complex ions dissociated from the electrolyte, and the electropositive aluminum complex ions are AlCl2 +、AlCl2 +Or Al3+(ii) a During charging, electronegative cyano organic molecules are dissociated from electropositive aluminum complex ions and are reoxidized into electroneutral organic matters; the discharging and charging voltage ranges of the metal aluminum-cyano organic matter battery are 0.8-2.0V and 1.0-2.2V respectively, and the charging and discharging current density ranges are 0.01-10A g-1Specific capacity of 50-300mAh g-1。
2. The method of claim 1, wherein the organic positive electrode having a cyano group is one or more selected from benzonitrile, cinnamonitrile, 4-pyridylacetonitrile, diphenylacetonitrile, 4-cyanobiphenyl, 1-naphthonitrile, 2-naphthonitrile, 10, 11-dihydro-5H-dibenzo [ a, D ] cycloheptene-5-carbonitrile, and 6-cyanoquinoline; the positive electrode of the organic matter containing two cyano groups is one or more than two of 1, 4-benzenediacetonitrile, phthalonitrile, 2-cyanophenylacetonitrile naphthalene-1, 4-dinitrile, 9, 10-dicyanoanthracene and m-phthalonitrile; the organic positive electrode containing three cyano groups is one or more than two of (benzene-1, 3, 5-triacyl) acetonitrile, 1,3, 5-tri (4-cyanophenyl) benzene, [1,3, 5-tri (4-cyanoethyl benzene) benzene and 2,4, 6-tricyano-1, 3, 5-trimethylbenzene; the organic positive electrode containing four cyano groups is one or more than two of 5,10,15, 20-tetra (4-cyanophenyl) porphyrin, 7,8, 8-tetracyano-p-quinodimethane, tetra (4-cyanophenyl) methane, tetracyanoethylene and 1,2,4, 5-benzene tetracyanonitrile; the organic positive electrode containing six cyano groups is hexacyanohexatriphenylene.
3. The method of claim 1, wherein the negative electrode is elemental aluminum or a binary or multicomponent alloy of aluminum and copper, iron, nickel, lead, bismuth, tin, silver.
4. The method of claim 1, wherein the mass ratio of the cyanoorganic material to the conductive additive to the binder is (6-8): 3-1): 1.
5. The method according to claim 4, wherein the conductive additive is one or more of acetylene black, graphite powder, carbon nanotubes and graphene.
6. The method of claim 1, wherein the conductive current collector is one of a tantalum sheet, a tantalum mesh, and a carbon cloth.
7. The method according to claim 1, wherein the aluminum chloride-inorganic acid salt electrolyte is one of aluminum chloride-triethylamine hydrochloride, aluminum chloride-1-butyl-3-methylimidazole chloride and aluminum chloride-phenyltrimethylammonium chloride, and a molar ratio of aluminum chloride to the inorganic acid salt in the electrolyte is 1: 1-3: 1.
8. The method of claim 1, wherein the solvent is one or a mixture of two or more of N-methylpyrrolidone, N-dimethylformamide, N-dimethylacetamide and dimethylsulfoxide.
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