CN110862111B - Preparation method of carbon-coated Co and Ni composite oxide nanoparticles - Google Patents
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Abstract
The invention discloses a preparation method of carbon-coated Co and Ni composite oxide nanoparticles, wherein cobalt acetate-tetrahydrate and nickel acetate-tetrahydrate are used as main raw materials, a proper amount of high-molecular PVP is added as a binder, an electrostatic spinning product is prepared under a high-pressure condition by using an electrostatic spinning technology, and then the electrostatic spinning product is sintered in a muffle furnace under a program temperature control condition to obtain the carbon-coated Co and Ni composite oxide nanoparticles which are used as a negative electrode material of a lithium ion battery and have good electrochemical performance; the nano-particles are used as a catalyst and have good catalytic performance. In the whole preparation process, the method is simple to operate, low in cost and low in equipment investment, meets the requirements of scientific development and sustainable development of the green environmental protection development concept, and is suitable for batch production.
Description
Technical Field
The invention belongs to the field of material chemistry, and particularly relates to a preparation method of carbon-coated Co and Ni composite oxide nanoparticles.
Background
After decades of rapid development of human society, energy shortage and environmental pollution become two major problems in the world, countries in the world begin to recognize the severity and urgency of the problems, and a discussion agenda is provided for solving the two problems, and the main methods for solving the problems are to increase the development and utilization of clean and renewable energy sources, replace fossil fuels with renewable clean energy sources, reduce the dependence on the fossil fuels, the clean and renewable energy sources include solar energy, wind energy, geothermal energy and tidal energy, nuclear energy and the like, which have the advantages of inexhaustible resources and no pollution to the environment, and have the disadvantages of being easily influenced by uncontrollable environmental factors such as seasonality, regionality, instability and the like, and greatly limiting the popularization and application of the nuclear energy and the like, so that the research on a reliable and stable energy storage and conversion device becomes one of the key technologies. In energy storage and conversion devices, secondary lithium ion batteries are excellent in energy storage and release processes, and thus have received wide attention from researchers. In 1979, the nose precursor of lithium batteries, dr.goodenough, discovered that lithium cobaltate was used as a positive electrode of the batteries, and a metal material other than lithium was used as a negative electrode, thereby enabling high-density energy storage, and then in 1980, dr.goodenough invented a cobalt oxide positive electrode, which is now used in all portable electronic devices around the world, and thus, dr.goodenough also acquired the nobel prize in 2019. As a novel and environment-friendly renewable energy storage device, a lithium ion battery has been widely used as a power source for various electric devices, as small as various portable electronic devices such as mobile phones and notebook computers, and as large as vehicles such as electric automobiles and light rail cloud rails, and the lithium ion battery affects the life of people all the time, thereby providing great convenience for human life.
In the charge-discharge cycle process of a secondary lithium ion battery, an efficient electrode material is of great importance, the electrode material with the nano structure can shorten an ion migration path and improve the migration rate of ions, and the active sites can be increased by a larger specific surface area to improve the electrochemical reaction activity of the material. The nano material has the advantages of directional electron and ion conduction directions, short radial ion transmission path, strong stress bearing capacity, large electrochemical active surface area and the like, so that the nano material becomes an electrode material with a very promising prospect.
The electrostatic spinning Technology utilizes electrostatic field force, and is simple in operation and controllable in method, so that various inorganic carbon-containing nano materials, such as carbon materials, metal oxides, phosphide, sulfides and the like, are prepared, the obtained composite material has good conductivity and a rapid electron ion transmission path, and therefore, the composite material is widely used for secondary battery electrode materials, and Huang ZM et al (Composites Science and Technology,2003,63: 2223-: the spinning nozzle, the high-voltage power supply and the collecting device; (ii) a In the electrostatic spinning process, when high voltage is applied between a spinneret and a receiving plate, the solution sprayed from a needle head is subjected to electrostatic field force and solution surface tension at the same time, when the electrostatic field force and the surface tension applied to the liquid drops are balanced, a triangular cone type Taylor cone is formed at the needle head, and when the voltage is increased, the electrostatic field force of the liquid drops is greater than the surface tension, the liquid drops are stretched into fibers and are continuously sprayed on the receiving plate under the action of the electrostatic field force; the factors influencing the morphology of the electrostatic spinning fiber mainly comprise the following aspects: (1) system parameters such as molecular weight and purity of the polymer, conductivity, viscosity, dielectric constant, etc. of the precursor solution; (2) operating parameters such as gauge of the needle, voltage, rate of advancement, distance between the spinneret and the collector; (3) environmental parameters such as humidity, temperature, etc.; in addition, parameters in the annealing process of the spinning fiber, such as calcination temperature, calcination atmosphere, heating rate and the like, have relatively large influence on the structure, the appearance and the performance of the nanofiber material. Dan Li et al (advanced Materials,2004,16: 1151-.
At present, marketThe lithium ion battery cathode material commonly used in the field is mainly a carbon material, and comprises natural graphite, synthetic graphite, carbon fiber, mesophase spherule carbon and the like; the theoretical specific capacity of carbon is 372mAh g-1Carbon materials are widely used as negative electrode materials of commercial lithium ion batteries due to the advantages of low price, abundant resources and the like, but the graphite negative electrode battery can generate structural damage in the circulating process, an SEI (solid electrolyte interphase) film is easy to generate, irreversible capacity loss is caused by lithium precipitation, and the requirements of high multiplying power and long service life of the electrode materials are difficult to meet. Kazunori et al (Materials Transactions, JIM,2000,41,1621-0.5Ni0.5The chemical activity of O, thus the idea is that the carbon-coated bimetallic oxide Co is prepared by adopting the electrostatic spinning technology0.5Ni0.5The O composite oxide nano-particle material relieves the volume expansion effect of the bimetallic oxide in the charging and discharging processes, overcomes the defects of low theoretical specific capacity of the carbon material, easy formation of SEI (solid electrolyte interphase) film and the like, combines the advantages of the two materials through an electrochemical performance test, effectively improves the electrochemical performance of the material, and has higher cyclic specific capacity, stable structure and good reversibility.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of carbon-coated Co and Ni composite oxide nanoparticles in the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of carbon-coated Co and Ni composite oxide nanoparticles comprises the following steps of taking cobalt acetate tetrahydrate and nickel acetate tetrahydrate as main raw materials, adding a proper amount of macromolecules as an adhesive, magnetically stirring for a period of time to obtain a clear and transparent spinning precursor solution, preparing an electrostatic spinning product under a high voltage condition by using an electrostatic spinning technology, and sintering at 450-600 ℃ in a muffle furnace under the air condition to obtain the carbon-coated Co and Ni composite oxide nanoparticles, wherein the preparation method comprises the following steps:
(1) weighing a proper amount of cobalt acetate-tetrahydrate and nickel acetate-tetrahydrate, dissolving the cobalt acetate-tetrahydrate and the nickel acetate-tetrahydrate in a proper amount of a mixture solvent of N, N-Dimethylformamide (DMF) and absolute ethyl alcohol in a volume ratio of 1:1, stirring for 30min, adding a proper amount of PVP (K-13, polyvinylpyrrolidone), continuously stirring for 2h, and adjusting the pH value of the mixed solution to 4.5-6.5 by using glacial acetic acid to obtain a clear and transparent spinning precursor mixed solution;
(2) injecting the clear and transparent spinning precursor mixed solution into a 10mL injector, wherein the voltage is 16-19 kV, the distance between a needle head and a receiver is 15-20 cm, and the propelling flow rate is 1.2mL h-1Carrying out electrostatic spinning at the temperature of 35 ℃ and the humidity of 30% to obtain an electrostatic spinning product;
(3) placing the electrostatic spinning product in a crucible of a muffle furnace, heating to 200-300 ℃ for 180min in the air atmosphere, sintering for 3h, and then carrying out N2Heating to 500-600 ℃ in 120min in the atmosphere, sintering for 2h, and naturally cooling to room temperature to obtain carbon-coated Co and Ni composite oxide nanoparticles;
the PVP is K-13 type polyvinylpyrrolidone; the DMF is N, N-dimethylformamide;
the mass ratio of Co (II) ions to Ni (II) ions in the mixed solution is 1: 1;
the concentration of Co (II) ions in the mixed solution is 0.1 mmol/mL;
the concentration of Ni (II) ions in the mixed solution is 0.1 mmol/mL;
the concentration of PVP in the mixed solution is 1.5 g/mL;
the mass percentage of carbon in the carbon-coated Co and Ni composite oxide nanoparticles is 3-10%;
the chemical formula of the carbon-coated Co and Ni composite oxide nano-particles is simply Co0.5Ni0.5O@C。
The carbon-coated Co and Ni composite oxide nano-particles are used as a lithium ion battery negative electrode material, and the current density is 100mA g-1Under the condition, the specific capacity of the first discharge is 625mAh g-1After circulating for 140 circles, the specific capacity can still be kept at 167mAh g-1Above that, the coulombic efficiency is kept above 98.5%.
In addition, the carbon-coated Co and Ni composite oxide nano-particles prepared by the preparation methodAs catalyst, 4-bromobenzaldehyde, ethyl acetoacetate and ammonium acetate AcONH4The yield of the 1, 4-dihydropyridine derivative is over 75 percent by taking ethanol and water with the volume ratio of 1:1 as a solvent and reacting at the temperature of 70 ℃.
Compared with the prior art, the composite oxide nano-particles synthesized by the invention have the following characteristics:
(1) by combining electrostatic spinning and programmed sintering technologies, the prepared oxide nanoparticles are uniform, have the diameter of 50-80 nm and large specific surface area, and are beneficial to improving the specific capacity of the material;
(2) the prepared oxide nano-particles are doped with carbon, so that the volume expansion effect of the material can be slowed down, the conductivity of the material can be improved, and the Li in the charging and discharging process can be improved+The rate of intercalation and deintercalation;
(3) the bimetallic oxide Co0.5Ni0.5The O nano material has a composition structure which is easy to regulate, and the electrochemical performance of the material can be regulated and controlled by regulating and controlling the components of carbon and metal.
Drawings
FIG. 1 is an XRD pattern of composite oxide nanoparticles prepared according to the present invention;
FIG. 2 is an SEM image of composite oxide nanoparticles prepared according to the present invention;
fig. 3 is a graph of charge-discharge cycle and coulombic efficiency of the composite oxide nanoparticles prepared by the invention as a lithium ion battery negative electrode material.
Detailed Description
The present invention is further described in detail with reference to the following examples, and the technical solution of the present invention is not limited to the specific embodiments listed below, but includes any combination of the specific embodiments.
Example 1
1.0mmoL (0.249g) cobalt acetate tetrahydrate (C) was weighed4H6CoO4·4H2O) and 1.0mmoL (0.248g) Nickel acetate tetrahydrate (C)4H6NiO4·4H2O), dissolved in 5.0mL of DMF and 5.0mL of absolute ethanol, stirred for 30min,adding 1.5g of PVP (K-13 polyvinylpyrrolidone) and continuously stirring for 2h, and adjusting the pH value of the mixed solution to 4.5 by using glacial acetic acid to obtain a clear and transparent spinning precursor mixed solution; injecting the clear and transparent spinning precursor mixed solution into a 10mL injector, wherein the voltage is 16kV, the vertical distance between a needle head and a receiver is 15cm, and the propelling flow rate is 1.2mL h-1Carrying out electrostatic spinning at the temperature of 35 ℃ and the humidity of 30% to obtain a spinning product; placing the electrostatic spinning product in a crucible of a muffle furnace, heating to 200 ℃ for 180min in air atmosphere, sintering for 3h, and then performing N2Heating to 500 ℃ in 120min in the atmosphere, sintering for 2h, and then naturally cooling to room temperature to obtain the black carbon-coated Co and Ni composite oxide nanoparticle product; the product is subjected to X-ray powder diffraction analysis, and the composition structure of the product is tested (figure 1); observing the shape of the nano-particle type nano-particle with a scanning electron microscope, wherein the diameter of the nano-particle is 50-80 nm (shown in figure 2); the mass percentage of carbon in the product is 10 percent by element analysis and test; the prepared composite oxide nano-particles are used as the negative electrode material of the lithium ion battery, and the current density is 100mA g-1First discharge specific capacity 625mAh g-1After circulating for 140 circles, the specific capacity can still be kept at 167mAh g-1Above, the coulombic efficiency remained above 98.5% (fig. 3).
Example 2
1.0mmoL (0.249g) cobalt acetate tetrahydrate (C) was weighed4H6CoO4·4H2O) and 1.0mmoL (0.248g) Nickel acetate tetrahydrate (C)4H6NiO4·4H2O), dissolving in 5.0mL of DMF and 5.0mL of absolute ethanol, stirring for 30min, adding 1.5g of PVP (K-13 polyvinylpyrrolidone), continuously stirring for 2h, and adjusting the pH value of the mixed solution to 6.5 by using glacial acetic acid to obtain a clear and transparent spinning precursor mixed solution; injecting the clear and transparent spinning precursor mixed solution into a 10mL injector, wherein the voltage is 19kV, the vertical distance between a needle head and a receiver is 20cm, and the propelling flow rate is 1.2mL h-1Carrying out electrostatic spinning at the temperature of 35 ℃ and the humidity of 30% to obtain a spinning product; placing the electrostatic spinning product in a crucible of a muffle furnace in an air atmosphereUnder the atmosphere, the temperature is raised to 300 ℃ for 180min and the mixture is sintered for 3h, and then the mixture is sintered in N2Heating to 600 ℃ in 120min in the atmosphere, sintering for 2h, and naturally cooling to room temperature to obtain the black carbon-coated Co and Ni composite oxide nanoparticle product; the mass percentage of carbon in the product is 3 percent by element analysis and test; analyzing the composition structure and the morphology of the product by X-ray powder diffraction and SEM test; the electrochemical performance of the product was tested with an electrochemical test system.
Example 3
1.0mmoL (0.249g) cobalt acetate tetrahydrate (C) was weighed4H6CoO4·4H2O) and 1.0mmoL (0.248g) Nickel acetate tetrahydrate (C)4H6NiO4·4H2O), dissolving in 5.0mL of DMF and 5.0mL of absolute ethanol, stirring for 30min, adding 1.5g of PVP (K-13 polyvinylpyrrolidone), continuously stirring for 2h, and adjusting the pH value of the mixed solution to 5.5 by using glacial acetic acid to obtain a clear and transparent spinning precursor mixed solution; injecting the clear and transparent spinning precursor mixed solution into a 10mL injector, wherein the voltage is 18kV, the vertical distance between a needle head and a receiver is 17cm, and the propelling flow rate is 1.2mL h-1Carrying out electrostatic spinning at the temperature of 35 ℃ and the humidity of 30% to obtain a spinning product; placing the electrostatic spinning product in a crucible of a muffle furnace, heating to 250 ℃ for 180min in air atmosphere, sintering for 3h, and then performing N2Heating to 550 ℃ in 120min in the atmosphere, sintering for 2h, and then naturally cooling to room temperature to obtain the black carbon-coated Co and Ni composite oxide nanoparticle product; the mass percentage of carbon in the product is 7 percent by element analysis test; analyzing the composition structure and the morphology of the product by X-ray powder diffraction and SEM test; the electrochemical performance of the product was tested with an electrochemical test system.
The prepared composite oxide nano-particles are used as a catalyst, and the product yield of the following reaction can be up to more than 75 percent: 20mL of solvent 20mL of ethanol and water with the volume ratio of 1:1, 1.0mmol of 4-bromobenzaldehyde, 2.0mmol of ethyl acetoacetate and 4.0mmol of ammonium acetate AcONH4As raw material, 1, 4-dihydropyridine derivative is generated at the reaction temperature of 70 ℃,the reaction equation is as follows:
Claims (1)
1. a preparation method of carbon-coated Co and Ni composite oxide nanoparticles is characterized by comprising the following steps:
(1) weighing cobalt acetate-tetrahydrate and nickel acetate-tetrahydrate, dissolving the cobalt acetate-tetrahydrate and the nickel acetate-tetrahydrate in a mixture solvent of N, N-dimethylformamide and absolute ethyl alcohol in a volume ratio of 1:1, stirring for 30min, adding a proper amount of PVP, continuously stirring for 2h, and adjusting the pH value of the mixed solution to 4.5-6.5 by using glacial acetic acid to obtain a clear and transparent spinning precursor mixed solution;
(2) injecting the clear and transparent spinning precursor mixed solution into a 10mL injector, wherein the voltage is 16-19 kV, the distance between a needle head and a receiver is 15-20 cm, and the propelling flow rate is 1.2mL h-1Carrying out electrostatic spinning at the temperature of 35 ℃ and the humidity of 30% to obtain an electrostatic spinning product;
(3) placing the electrostatic spinning product in a crucible of a muffle furnace, heating to 200-300 ℃ for 180min in the air atmosphere, sintering for 3h, and then carrying out N2Heating to 500-600 ℃ in 120min in the atmosphere, sintering for 2h, and naturally cooling to room temperature to obtain carbon-coated Co and Ni composite oxide nanoparticles;
the carbon-coated Co and Ni composite oxide nano-particles are used as a lithium ion battery cathode material and have a current density of 100mA g-1Under the condition, the specific capacity of the first discharge is 625mAh g-1After circulating for 140 circles, the specific capacity can still be kept at 167mAh g-1Above, the coulombic efficiency is kept above 98.5%;
the carbon-coated Co and Ni composite oxide nanoparticles are used as a catalyst, 4-bromobenzaldehyde, ethyl acetoacetate and ammonium acetate are used as raw materials, ethanol and water in a volume ratio of 1:1 are used as solvents, and the yield of the 1, 4-dihydropyridine derivative is over 75% at the reaction temperature of 70 ℃;
the PVP is K-13 type polyvinylpyrrolidone;
the mass ratio of Co (II) ions to Ni (II) ions in the mixed solution is 1: 1;
the concentration of PVP in the mixed solution is 1.5 g/mL;
the mass percentage of carbon in the carbon-coated Co and Ni composite oxide nanoparticles is 3-10%;
the chemical formula of the carbon-coated Co and Ni composite oxide nano-particles is simply Co0.5Ni0.5O@C。
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