CN108448165B - Dual-ion battery adopting ternary composite material as negative electrode and preparation method thereof - Google Patents
Dual-ion battery adopting ternary composite material as negative electrode and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a double-ion battery using a ternary composite material as a negative electrode and a preparation method thereof. The preparation method disclosed by the invention is simple, green and environment-friendly, the raw materials are simple and easy to obtain, the cycle performance under large current is good, and the coulomb efficiency is high.
Description
Technical Field
The invention belongs to the field of electrochemical energy storage, particularly relates to a double-ion battery using a ternary composite material as a negative electrode and a preparation method thereof, and particularly relates to a double-ion battery using a metal/carbon/graphene ternary composite material as a negative electrode and a preparation method thereof.
Background
The lithium ion battery has the outstanding advantages of high specific energy density, long cycle life, small environmental pollution, no memory effect and the like, and has great success in the electronic field. However, the lithium metal is stored in the earth crust in a low amount and is not distributed uniformly, so that the manufacturing cost of the lithium ion battery is high, and therefore, the development of an energy storage technology with excellent performance, rich resources and low price is urgently needed. Among them, a bi-ion battery is emerging in recent years.
The double-ion battery has the advantages of higher working voltage, excellent specific energy density, low manufacturing cost and the like, is a new generation of high-performance power battery, is expected to break through the bottleneck of the development of new energy vehicles including Electric Vehicles (EV), gasoline-electric Hybrid Electric Vehicles (HEV) and plug-in hybrid electric vehicles (PHEV), and has only L i compared with the lithium ion battery+The two different ions of the double-ion battery participate in the reaction between the positive electrode and the negative electrode, and when the double-ion battery is charged, the metal salt (such as L iPF) in the electrolyte6，NaClO4Etc.) moves to the positive electrode, intercalation occurs at the positive electrodeCarrying out an insertion or adsorption reaction, wherein cations of the metal salt move to the negative electrode, an insertion or adsorption reaction occurs at the negative electrode, and accordingly, an external current flows from the negative electrode to the positive electrode; during discharging, anions and cations are respectively desorbed or desorbed from the positive electrode and the negative electrode and return to the electrolyte, and accordingly, current flows from the positive electrode to the negative electrode through an external load.
Currently, the most used negative electrode materials in the bi-ion battery are of two types, one is a metal-based material, such as aluminum foil, tin foil, and the like. During charging, the alloy type intercalation reaction can be carried out with metal salt cations, the theoretical specific capacity is high, but the metal can generate huge volume change in the alloying and dealloying circulating process, and the problems of unstable electrode material structure, serious pulverization, failure, poor circulating performance and the like can be caused. Another class is pure carbon-based materials, such as graphite, expanded graphite, graphene, and soft carbon, where metal cations can undergo intercalation mechanism or adsorption type reactions. The carbon material has good electronic conductivity, small volume change when metal ions are de-intercalated, is an ideal stable carrier, and has the advantages of low price, environmental protection and the like, but the theoretical specific capacity is low, and the multiplying power performance is poor. In conclusion, it is very necessary to find a composite material having the advantages of high theoretical specific capacity, high discharge medium voltage, small volume change during metal ion extraction and the like as a negative electrode material of a dual-ion battery.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a bi-ion battery using a ternary composite material as a negative electrode and a method for preparing the same, and more particularly, to a bi-ion battery using a metal/carbon/graphene ternary composite material as a negative electrode and a method for preparing the same, so as to solve the above existing problems and obtain a bi-ion battery having advantages of high specific energy density, long cycle life, excellent rate capability, excellent safety performance, and the like.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a metal/carbon/graphene ternary composite material is prepared by adopting a one-step high-temperature carbothermic method, the metal/carbon/graphene ternary composite material is used as a negative electrode, a graphite material is used as a positive electrode, and a metal salt electrolyte is assembled into the double-ion battery.
The invention also discloses a preparation method of the double-ion battery using the ternary composite material as the cathode, which comprises the following steps:
(1) dissolving metal salt, reducing organic acid and various nitrogen sources into a suspension solution of graphene oxide, performing dehydration treatment to obtain a precursor, and performing high-temperature carbonization treatment on the precursor to obtain a metal/carbon/graphene ternary composite material with metal particles embedded in a nitrogen-doped carbon matrix;
(2) and assembling the metal/carbon/graphene ternary composite material cathode, the graphite material anode and the metal salt electrolyte into the dual-ion battery.
In the method, the metal salt is one or more of metal zinc salt, metal antimony salt, metal lead salt and metal tin salt; the metal zinc salt is one or more of zinc chloride, zinc nitrate, zinc acetate and zinc sulfate; the metal antimony salt is one or more of antimony trichloride, antimony bromide, antimony pentachloride and antimony sulfate; the metal lead salt is one or more of lead nitrate and lead acetate; the metallic tin salt is one or more of stannous chloride, stannous nitrate, stannic chloride and stannous oxalate; the reducing organic acid is one or more of tartaric acid, citric acid and gluconic acid; the nitrogen source is one or more of melamine, cyanamide, urea and ammonium sulfate.
In the above process, the molar ratio of the metal salt to the reducing organic acid is (5 to 90): 100, preferably (10-70): 100, respectively; the molar ratio of the reducing organic acid to the nitrogen source is (10-90): 100, preferably (15-70): 100, respectively; the mass ratio of the graphene oxide to the metal salt is 1: (3-10).
In the method, the high-temperature carbonization treatment is to perform carbonization treatment on the precursor for 15-180min, preferably 20-120min at the high temperature of 400-1200 ℃, preferably at the temperature of 500-1000 ℃ under the protection of argon gas.
In the above method, the metal salt electrolyte is selected from one or more of lithium perchlorate, sodium perchlorate, potassium perchlorate, lithium hexafluorophosphate, sodium hexafluorophosphate and potassium hexafluorophosphate.
In the method, the voltage of the double-ion battery is 1.0-5.5V.
Compared with the prior art, the invention has the following excellent effects:
firstly, metal salt, reducing organic acid, various nitrogen sources and graphene oxide are selected as raw materials, and the metal (zinc, antimony, lead or tin and the like)/carbon/graphene ternary composite material can be prepared under the same test conditions. Therefore, the raw materials have larger selection space, are simple and easy to obtain, and have high coulombic efficiency. The whole synthesis process is very simple, time-saving, safe, low in cost, green and environment-friendly, and is suitable for large-batch industrial production; and secondly, the prepared ternary composite material metal (zinc, antimony, lead or tin and the like)/carbon/graphene with metal particles embedded into the nitrogen-doped carbon matrix is used as the cathode material of the double-ion battery, so that the synergistic effect among the components is utilized, and the purpose of complementary advantages among different components is achieved. The metal particles (zinc, antimony, lead or tin and the like) are high in potential of metal ions in the de-intercalation electrolyte, so that the generation of metal dendrites of the negative electrode can be effectively avoided, and the safety performance of the dual-ion battery is greatly improved. The carbon matrix is used as a carrier of the metal particles, so that the volume change of the metal particles in the repeated charge and discharge process can be buffered, and the circulation stability of the bi-ion battery under large current is improved. The theoretical specific capacity of metal (zinc, antimony, lead or tin and the like) is generally higher, and meanwhile, the carbon matrix can reduce the interface contact resistance among metal particles, so that the rate capability of the double-ion battery is effectively improved.
Drawings
The following is further described with reference to the accompanying drawings:
fig. 1 is a negative electrode X-ray powder diffraction pattern of the metallic antimony/carbon/graphene ternary composite provided in example 1:
fig. 2 is a TEM electron microscopic view of the metallic antimony/carbon/graphene ternary composite material cathode provided in example 1:
fig. 3 is an HRTEM electron microscopic view of the metallic antimony/carbon/graphene ternary composite negative electrode provided in example 1:
fig. 4 is a long-term charge-discharge cycle plot of the sodium bi-ion battery provided in example 1 at a current density of 1A/g:
fig. 5 is a graph of rate performance of the sodium bi-ion battery provided in example 1 at different current densities.
Detailed Description
The process of the present invention is illustrated below by means of specific examples, but the present invention is not limited thereto.
The experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Example 1: preparation method of sodium dual-ion battery
Sequentially dissolving antimony trichloride, citric acid and cyanamide into a certain amount of graphene oxide suspension solution, then performing dehydration treatment to obtain a high-temperature carbonized precursor, and finally performing carbonization treatment for 40min at a high temperature of 700 ℃ in a tubular furnace under the protection of argon atmosphere to obtain the metallic antimony/carbon/graphene ternary composite material cathode.
The sodium double-ion battery is manufactured in a glove box, wherein the positive electrode is commercial expanded graphite, the negative electrode is a metal antimony/carbon/graphene ternary composite material negative electrode, and the electrolyte is 1M sodium perchlorate (NaClO)4) The separator is a commercially available separator. The voltage of the double-ion battery is 2V-4.7V.
The metal antimony/carbon/graphene ternary composite material cathode is identified to be composed of pure metal antimony and amorphous carbon without any other impurity phase by an X-ray powder diffractometer (as shown in figure 1). The morphology was characterized by TEM (as shown in figure 2) and it was seen that the metallic antimony particles were embedded in the carbon matrix. Further HRTEM characterization (as shown in FIG. 3) can clearly see the lattice fringes of the metal antimony, and the measurement of the lattice fringe spacing of 0.31nm exactly corresponds to the (012) crystal plane spacing of the metal antimony, which proves that the metal antimony is successfully reduced by carbon heat.
As shown in fig. 4 to 5, the electrochemical performance of the sodium-ion bi-ion battery was investigated using the cycle stability performance, rate performance, and the like. FIG. 4 shows the long-term cycling stability of the Na-Bi-ion battery under a large current density of 1A/g, wherein the Na-Bi-ion battery still maintains a high specific discharge capacity of 73 mA h/g after 1400 cycles of charge and discharge, and the coulomb efficiency is continuously and stably maintained above 98% after 32 cycles. FIG. 5 shows the rate capability of the Na-based bi-ion battery under different current densities, and it can be seen from the graph that the specific discharge capacity of the battery can reach 178 mA h/g under a small current density (200 mA/g). Even under the high current density of 2A/g, the battery still has high discharge specific capacity of 62 mA h/g. Therefore, the sodium double-ion battery prepared by adopting the metallic antimony/carbon/graphene ternary composite material as the negative electrode material has excellent specific discharge capacity and super-good long-term cycling stability.
Example 2: preparation method of potassium double-ion battery
And (2) dissolving tin tetrachloride, tartaric acid and melamine into a certain amount of graphene oxide suspension solution in sequence, then performing dehydration treatment to obtain a high-temperature carbonized precursor, and finally performing carbonization treatment for 50min at high temperature of 900 ℃ in a tubular furnace protected by argon atmosphere to obtain the metallic tin/carbon/graphene ternary composite material cathode.
The potassium double-ion battery is manufactured in a glove box, wherein the positive electrode is commercial expanded graphite, the negative electrode is a metallic tin/carbon/graphene ternary composite material negative electrode, and the electrolyte is 1M potassium perchlorate (KClO)4) The separator is a commercially available separator. The voltage of the double-ion battery is 2V-5V.
Example 3: preparation method of lithium double-ion battery
Sequentially dissolving zinc chloride, gluconic acid and cyanamide into a certain amount of graphene oxide suspension solution, then performing dehydration treatment to obtain a high-temperature carbonized precursor, and finally performing carbonization treatment at a high temperature of 600 ℃ for 20min in a tubular furnace under the protection of argon atmosphere to obtain the metal zinc/carbon/graphene ternary composite material cathode.
The lithium double-ion battery is manufactured in a glove box, wherein the positive electrode is commercial expanded graphite, the negative electrode is a metal zinc/carbon/graphene ternary composite material negative electrode, and the electrolyte is 1M lithium perchlorate (L iClO)4) The separator is a commercially available separator. The voltage of the double-ion battery is 3V-5V.
Example 4: preparation method of lithium double-ion battery
Sequentially dissolving antimony trichloride, tartaric acid and urea into a certain amount of graphene oxide suspension solution, then performing dehydration treatment to obtain a high-temperature carbonized precursor, and finally performing carbonization treatment for 30min at a high temperature of 700 ℃ in a tubular furnace protected by argon atmosphere to obtain the metallic antimony/carbon/graphene ternary composite material cathode.
The lithium double-ion battery is manufactured in a glove box, wherein the positive electrode is commercial expanded graphite, the negative electrode is a metal antimony/carbon/graphene ternary composite material negative electrode, and the electrolyte is 1M lithium hexafluorophosphate (L iPF)6) The separator is a commercially available separator. The voltage of the double-ion battery is 3V-5V.
Example 5: preparation method of sodium dual-ion battery
Sequentially dissolving lead acetate, tartaric acid and melamine into a certain amount of graphene oxide suspension solution, then performing dehydration treatment to obtain a high-temperature carbonized precursor, and finally performing carbonization treatment for 50min at a high temperature of 800 ℃ in a tubular furnace protected by argon atmosphere to obtain the metallic lead/carbon/graphene ternary composite material cathode.
The sodium double-ion battery is manufactured in a glove box, wherein the positive electrode is commercial expanded graphite, the negative electrode is a metal lead/carbon/graphene ternary composite material negative electrode, and the electrolyte is 1M sodium hexafluorophosphate (NaPF)6) The separator is a commercially available separator. The voltage of the double-ion battery is 1.5V-5V.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (5)
1. A bi-ion battery using a ternary composite material as a cathode is characterized in that the metal/carbon/graphene ternary composite material is prepared by a one-step high-temperature carbothermic method, the metal/carbon/graphene ternary composite material is used as the cathode, a graphite material is used as an anode, and a metal salt electrolyte is assembled into the bi-ion battery; the preparation method comprises the following steps:
(1) dissolving metal salt, reducing organic acid and various nitrogen sources into a suspension solution of graphene oxide, performing dehydration treatment to obtain a precursor, and performing high-temperature carbonization treatment on the precursor to obtain a metal/carbon/graphene ternary composite material with metal particles embedded in a nitrogen-doped carbon matrix;
(2) assembling a metal/carbon/graphene ternary composite material cathode, a graphite material anode and a metal salt electrolyte into a dual-ion battery;
the metal salt is one or more of metal zinc salt, metal antimony salt, metal lead salt and metal tin salt; the metal zinc salt is one or more of zinc chloride, zinc nitrate, zinc acetate and zinc sulfate; the metal antimony salt is one or more of antimony trichloride, antimony bromide, antimony pentachloride and antimony sulfate; the metal lead salt is one or more of lead nitrate and lead acetate; the metallic tin salt is one or more of stannous chloride, stannous nitrate, stannic chloride and stannous oxalate;
the reducing organic acid is one or more of tartaric acid, citric acid and gluconic acid; the nitrogen source is one or more of melamine, cyanamide, urea and ammonium sulfate;
the molar ratio of the metal salt to the reducing organic acid is (5-90): 100, respectively; the molar ratio of the reducing organic acid to the nitrogen source is (10-90): 100, respectively; the mass ratio of the graphene oxide to the metal salt is 1: (3-10);
the high-temperature carbonization treatment is to perform carbonization treatment on the precursor for 15-180min at the high temperature of 400-1200 ℃ under the protection atmosphere of argon;
the metal salt electrolyte is selected from one or more of lithium perchlorate, sodium perchlorate, potassium perchlorate, lithium hexafluorophosphate, sodium hexafluorophosphate and potassium hexafluorophosphate.
2. The method of manufacturing a bi-ion battery of claim 1, comprising the steps of:
(1) dissolving metal salt, reducing organic acid and various nitrogen sources into a suspension solution of graphene oxide, performing dehydration treatment to obtain a precursor, and performing high-temperature carbonization treatment on the precursor to obtain a metal/carbon/graphene ternary composite material with metal particles embedded in a nitrogen-doped carbon matrix;
(2) assembling a metal/carbon/graphene ternary composite material cathode, a graphite material anode and a metal salt electrolyte into a dual-ion battery;
the metal salt is one or more of metal zinc salt, metal antimony salt, metal lead salt and metal tin salt; the metal zinc salt is one or more of zinc chloride, zinc nitrate, zinc acetate and zinc sulfate; the metal antimony salt is one or more of antimony trichloride, antimony bromide, antimony pentachloride and antimony sulfate; the metal lead salt is one or more of lead nitrate and lead acetate; the metallic tin salt is one or more of stannous chloride, stannous nitrate, stannic chloride and stannous oxalate;
the reducing organic acid is one or more of tartaric acid, citric acid and gluconic acid; the nitrogen source is one or more of melamine, cyanamide, urea and ammonium sulfate;
the molar ratio of the metal salt to the reducing organic acid is (5-90): 100, respectively; the molar ratio of the reducing organic acid to the nitrogen source is (10-90): 100, respectively; the mass ratio of the graphene oxide to the metal salt is 1: (3-10);
the high-temperature carbonization treatment is to perform carbonization treatment on the precursor for 15-180min at the high temperature of 400-1200 ℃ under the protection atmosphere of argon;
the metal salt electrolyte is selected from one or more of lithium perchlorate, sodium perchlorate, potassium perchlorate, lithium hexafluorophosphate, sodium hexafluorophosphate and potassium hexafluorophosphate.
3. The method of claim 2, wherein: the molar ratio of the metal salt to the reducing organic acid is (10-70): 100, respectively; the molar ratio of the reducing organic acid to the nitrogen source is (15-70): 100.
4. the method of claim 2, wherein: the high-temperature carbonization treatment is to perform carbonization treatment on the precursor for 20-120min at the high temperature of 500-1000 ℃ under the protection atmosphere of argon.
5. The method of claim 2, wherein: the voltage of the double-ion battery is 1.0-5.5V.
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