CN107394188B - Preparation method of hollow spherical niobium oxide electrode material for lithium ion battery - Google Patents

Preparation method of hollow spherical niobium oxide electrode material for lithium ion battery Download PDF

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CN107394188B
CN107394188B CN201710524784.1A CN201710524784A CN107394188B CN 107394188 B CN107394188 B CN 107394188B CN 201710524784 A CN201710524784 A CN 201710524784A CN 107394188 B CN107394188 B CN 107394188B
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lithium ion
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黄剑锋
仵婉晨
李嘉胤
曹丽云
吴建鹏
周磊
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Shaanxi University of Science and Technology
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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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • 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
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E60/10—Energy storage using batteries

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Abstract

A preparation method of a hollow spherical niobium oxide electrode material for a lithium ion battery comprises the steps of firstly, adding analytically pure niobium oxalate hydrate into a hydrochloric acid solution to obtain A; suspending rape pollen in hydrochloric acid solution to obtain B; washing B with water, washing with alcohol, placing in a culture dish, and adding hexadecyl trimethyl ammonium bromide to obtain C; adding the A and the C into a reaction kettle, sealing the reaction kettle, carrying out hydrothermal reaction in a homogeneous phase reactor, naturally cooling to room temperature after the reaction is finished, and precipitating; washing the precipitate with water and alcohol, placing the precipitate in a culture dish, and transferring the precipitate to a vacuum drier for vacuum drying to obtain D; taking the precursor D in a dry pot, carrying out heat treatment under the protection of oxygen, and then cooling along with a furnace to obtain a target product Nb2O5. The invention adopts a hydrothermal calcination combined method to efficiently and quickly prepare the hollow spherical Nb with uniform distribution and good crystallinity2O5And (4) crystals. Adopting rape pollen as Nb2O5The template has the advantages of simple production process, low cost, environmental protection and contribution to regulating and controlling the structure and the appearance of the prepared material.

Description

Preparation method of hollow spherical niobium oxide electrode material for lithium ion battery
Technical Field
The invention belongs to the technical field of battery materials, relates to a method for preparing a lithium ion battery anode material, and particularly relates to a method for preparing a hollow spherical niobium oxide electrode material for a lithium ion battery.
Background
As an efficient energy storage device, the lithium ion battery has high energy density, long service life, good safety performance and the like in the use process, can be used for multiple times, and has no pollution to the environment, so that the lithium ion battery is an ideal green chemical energy source [ Sun Lei, Qin Xiu Juan, Ph based Chi Ming, and the like ]. The structure of the lithium ion battery mainly comprises four parts: the positive electrode material, the electrolyte, the diaphragm and the negative electrode material account for the highest proportion of the electrode material in the manufacturing cost of the battery, and the electrode material is closely related to the specific capacity, the cycle service life and other performances of the battery, so the research on the electrode material is always a hot point of research in the research on the lithium ion battery.
Currently, the positive electrode material of the lithium ion battery is generally lithium cobalt oxide, lithium nickel oxide, lithium manganese oxide, manganese nickel cobalt composite oxide, lithium vanadium oxide, lithium iron oxide, and the like, and L iCoO is generally used as the positive electrode material of the lithium ion battery that has been commercialized2、LiNiO2、LiMn2O4、LiCoO2、LiMn2O4[ Zhanghui, Zhengdinggang, Lidecheng, etc. ] preparation of novel lithium battery positive electrode material and electrochemical performance research [ J]Power supply technology, 2013,37(3):366-]However, the theoretical capacity is smaller, the actual capacity is smaller, and a series of influences are generated in the using process. The cost of the positive electrode material in the manufacturing process of the lithium ion battery is the highest, the capacity of the positive electrode material is far lower than that of the negative electrode material, and meanwhile, the electrochemical performance of the lithium ion battery depends on the structure and the appearance of the positive electrode material to a great extent, so the positive electrode material becomes a hot spot for the research of the lithium ion battery in recent years. The Nb-based oxide has higher capacity and great potential as a positive electrode material of a lithium ion battery, and the Nb-based oxide mainly comprises the following components: nb2O5、NbO2、Nb2O3And NbO, wherein Nb2O5Is relatively most stable.
Dunn[Kim J W,Augustyn V,Dunn B.The effect of crystallinity on therapid pseudocapacitive response of Nb2O5[J].Advanced Energy Materials,2011,2(1):141-148]The research of the people shows that T-Nb2O5 has higher theoretical capacity and working potential window, Nb2O5 as the anode material of the battery hardly deforms in the charge-discharge cycle process of the battery, so the structure of the battery is hardly influenced [ Louis, Chengxiang, Mayulin, and the like]Chemical progression 2015,27(2):000297-]Compared with transmissionThe electrode material is an ideal battery anode material. But due to Nb2O5The conductivity of the material is poor, so that the discharge performance of the material with high multiplying power is limited, and therefore, the Nb content is improved2O5Change the reaction site, increase the specific surface area, and increase Nb2O5Rate capability and cycle capability of (a).
By controlling Nb2O5The structure morphology of can greatly improve Nb2O5Cycling stability of electrode materials, however, Nb is currently reported2O5Most of the shapes of the electrode are nano-rod-shaped, nano-particles, nano-block-shaped and the like, or a complex preparation process is needed, so that the production cost of the electrode material is greatly increased, and the electrode material is not beneficial to mass production. Therefore, the development of a special structure is beneficial to increasing Nb2O5The prepared Nb has the advantages of conductivity, low cost and simple and convenient process2O5The method of the electrode material is of great significance.
Disclosure of Invention
The invention aims to overcome the defects of the existing structure and provides a method for preparing a hollow spherical niobium oxide electrode material for a lithium ion battery by hydrothermal calcination and heat treatment. The method can be used for preparing the hollow spherical Nb with controllable appearance and uniform particle size2O5An electrode material. And the preparation process is simple, the reaction period is short, the cost is low, and the method has a wide development prospect.
In order to achieve the purpose, the invention adopts the technical scheme that:
1) firstly, 0.80-1.0g of analytically pure niobium oxalate hydrate is added into 30-70ml of hydrochloric acid solution with the concentration of 0.1-0.5mol/l, the mixture is uniformly stirred, and then the mixture is subjected to ultrasonic dispersion to obtain transparent solution A;
2) suspending 4.3-4.7g of rape pollen in 10-50ml of 0.2-0.7mol/l hydrochloric acid solution, and uniformly stirring to obtain a mixed solution B;
3) respectively washing the mixed solution B with water and alcohol, placing the washed mixed solution B into a culture dish, adding 0.5-1g of hexadecyl trimethyl ammonium bromide into the culture dish, and heating and uniformly stirring the mixture to obtain mixed solution C;
4) adding the obtained transparent solution A and the mixed solution C into a reaction kettle, sealing, carrying out hydrothermal reaction in a homogeneous reaction instrument, naturally cooling to room temperature after the reaction is finished, and precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, placing the washed precipitate in a culture dish, transferring the culture dish into a vacuum drier, and carrying out vacuum drying at the temperature of 100 ℃ to obtain a precursor D;
6) taking the precursor D in a dry pot, raising the temperature from room temperature to 500 ℃ and 600 ℃ at the heating rate of 5 ℃/min for processing for 5h under the protection of oxygen, and then cooling along with the furnace to obtain the target product Nb2O5。
The step 1) ultrasonic dispersion is carried out for 60-120 min.
The filling ratio in the reaction kettle in the step 4) is 30-60%, the reaction temperature of the homogeneous phase reactor is 80-120 ℃, and the reaction time is 11-15 h.
The invention has the beneficial effects that:
1) the hollow spherical Nb with uniform distribution and good crystallinity is efficiently and rapidly prepared by adopting a hydrothermal calcination combination method2O5And (4) crystals.
2) Adopting rape pollen as Nb2O5The template has the advantages of simple production process, low cost, environmental protection and contribution to regulating and controlling the structure and the appearance of the prepared material.
Drawings
FIG. 1 is a hollow spherical Nb prepared in example 12O5XRD pattern of electrode material.
FIG. 2 is a hollow spherical Nb prepared in example 12O5SEM photograph of the electrode material.
FIG. 3 is a hollowed-out spherical Nb prepared in example 12Graph of rate capability of O electrode material.
Detailed Description
Example 1:
1) firstly, adding 0.80g of analytically pure niobium oxalate hydrate into 30ml of hydrochloric acid solution with the concentration of 0.1mol/l, uniformly stirring, and then performing ultrasonic dispersion for 60min to obtain a transparent solution A;
2) suspending 4.3g of rape pollen in 10ml of hydrochloric acid solution with the concentration of 0.2mol/l, and uniformly stirring to obtain mixed solution B;
3) respectively washing the mixed solution B with water and alcohol, placing the washed mixed solution B in a culture dish, adding 0.5g of Cetyl Trimethyl Ammonium Bromide (CTAB), heating and uniformly stirring to obtain a mixed solution C;
4) adding the obtained transparent solution A and the mixed solution C into a reaction kettle, controlling the filling ratio to be 30%, sealing, carrying out hydrothermal reaction in a homogeneous reaction instrument, controlling the reaction temperature to be 80 ℃, reacting for 11h, naturally cooling to room temperature after the reaction is finished, and precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, placing the washed precipitate in a culture dish, transferring the culture dish into a vacuum drier, and carrying out vacuum drying at the temperature of 100 ℃ to obtain a precursor D;
6) taking the precursor D in a dry pot, raising the temperature from room temperature to 500 ℃ at the heating rate of 5 ℃/min under the protection of oxygen, treating for 5 hours, and then cooling along with a furnace to obtain a target product Nb2O5。
It can be seen from FIG. 1 that the combination of the thermal calcination method can successfully prepare Nb2O5An electrode material. Nb2O5Diffraction peak of (2) and 27-1003Nb2O5The standard cards correspond.
As can be seen from FIG. 2, Nb is produced2O5The composite electrode material is spherical with a plurality of hollow small holes and uniform size.
FIG. 3 is a prepared hollowed-out spherical Nb2The multiplying power performance pictures of the O electrode material show that the specific capacities of the products are respectively 220, 200, 190, 175, 157 mAh.g under the current densities of 50mA, 100mA, 200mA, 500mA and 1000mA-1(ii) a And when the current density returns to 50mA again, the specific capacity of the product can return to 217mAh g-1(98%) from this, Nb is observed2O5The rate capability of the anode material is more outstanding.
Example 2:
1) firstly, adding 0.85g of analytically pure niobium oxalate hydrate into 40ml of hydrochloric acid solution with the concentration of 0.2mol/l, uniformly stirring, and then performing ultrasonic dispersion for 80min to obtain a transparent solution A;
2) suspending 4.4g of rape pollen in 20ml of hydrochloric acid solution with the concentration of 0.3mol/l, and uniformly stirring to obtain mixed solution B;
3) respectively washing the mixed solution B with water and alcohol, placing the washed mixed solution B in a culture dish, adding 0.6g of Cetyl Trimethyl Ammonium Bromide (CTAB), heating and uniformly stirring to obtain a mixed solution C;
4) adding the obtained transparent solution A and the mixed solution C into a reaction kettle, controlling the filling ratio to be 35%, sealing, carrying out hydrothermal reaction in a homogeneous reaction instrument, controlling the reaction temperature to be 90 ℃, the reaction time to be 12h, naturally cooling to room temperature after the reaction is finished, and then precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, placing the washed precipitate in a culture dish, transferring the culture dish into a vacuum drier, and carrying out vacuum drying at the temperature of 100 ℃ to obtain a precursor D;
6) taking the precursor D in a dry pot, raising the temperature from room temperature to 525 ℃ at the heating rate of 5 ℃/min under the protection of oxygen, treating for 5 hours, and then cooling along with a furnace to obtain a target product Nb2O5。
Example 3:
1) firstly, adding 0.90g of analytically pure niobium oxalate hydrate into 50ml of hydrochloric acid solution with the concentration of 0.3mol/l, uniformly stirring, and then performing ultrasonic dispersion for 100min to obtain a transparent solution A;
2) suspending 4.5g of rape pollen in 30ml of hydrochloric acid solution with the concentration of 0.4mol/l, and uniformly stirring to obtain mixed solution B;
3) respectively washing the mixed solution B with water and alcohol, placing the washed mixed solution B in a culture dish, adding 0.7g of Cetyl Trimethyl Ammonium Bromide (CTAB), heating and uniformly stirring to obtain a mixed solution C;
4) adding the obtained transparent solution A and the mixed solution C into a reaction kettle, controlling the filling ratio to be 40%, sealing, carrying out hydrothermal reaction in a homogeneous reaction instrument, controlling the reaction temperature to be 100 ℃, the reaction time to be 13h, naturally cooling to room temperature after the reaction is finished, and then precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, placing the washed precipitate in a culture dish, transferring the culture dish into a vacuum drier, and carrying out vacuum drying at the temperature of 100 ℃ to obtain a precursor D;
6) taking the precursor D in a dry pot, raising the temperature from room temperature to 550 ℃ at the heating rate of 5 ℃/min under the protection of oxygen, treating for 5 hours, and then cooling along with a furnace to obtain a target product Nb2O5。
Example 4:
1) firstly, 0.95g of analytically pure niobium oxalate hydrate is added into 60ml of hydrochloric acid solution with the concentration of 0.4mol/l, the mixture is stirred uniformly, and then the mixture is subjected to ultrasonic dispersion for 110min to obtain transparent solution A;
2) suspending 4.6g of rape pollen in 40ml of hydrochloric acid solution with the concentration of 0.6mol/l, and uniformly stirring to obtain mixed solution B;
3) respectively washing the mixed solution B with water and alcohol, placing the washed mixed solution B in a culture dish, adding 0.8g of Cetyl Trimethyl Ammonium Bromide (CTAB), heating and uniformly stirring to obtain a mixed solution C;
4) adding the obtained transparent solution A and the mixed solution C into a reaction kettle, controlling the filling ratio to be 50%, sealing, carrying out hydrothermal reaction in a homogeneous reaction instrument, controlling the reaction temperature to be 110 ℃, reacting for 14h, naturally cooling to room temperature after the reaction is finished, and precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, placing the washed precipitate in a culture dish, transferring the culture dish into a vacuum drier, and carrying out vacuum drying at the temperature of 100 ℃ to obtain a precursor D;
6) taking the precursor D in a dry pot, raising the temperature from room temperature to 575 ℃ at the heating rate of 5 ℃/min for treatment for 5h under the protection of oxygen, and then cooling along with a furnace to obtain a target product Nb2O5。
Example 5:
1) firstly, adding 1.0g of analytically pure niobium oxalate hydrate into 70ml of hydrochloric acid solution with the concentration of 0.5mol/l, uniformly stirring, and then performing ultrasonic dispersion for 120min to obtain a transparent solution A;
2) suspending 4.7g of rape pollen in 50ml of hydrochloric acid solution with the concentration of 0.7mol/l, and uniformly stirring to obtain mixed solution B;
3) respectively washing the mixed solution B with water and alcohol, placing the washed mixed solution B in a culture dish, adding 1g of Cetyl Trimethyl Ammonium Bromide (CTAB), heating and uniformly stirring to obtain a mixed solution C;
4) adding the obtained transparent solution A and the mixed solution C into a reaction kettle, controlling the filling ratio to be 60%, sealing, carrying out hydrothermal reaction in a homogeneous reaction instrument, controlling the reaction temperature to be 120 ℃, the reaction time to be 15h, naturally cooling to room temperature after the reaction is finished, and then precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, placing the washed precipitate in a culture dish, transferring the culture dish into a vacuum drier, and carrying out vacuum drying at the temperature of 100 ℃ to obtain a precursor D;
6) taking the precursor D in a dry pot, raising the temperature from room temperature to 600 ℃ at the heating rate of 5 ℃/min under the protection of oxygen, treating for 5 hours, and then cooling along with a furnace to obtain a target product Nb2O5。

Claims (3)

1. A preparation method of a hollow spherical niobium oxide electrode material for a lithium ion battery is characterized by comprising the following steps:
1) firstly, 0.80-1.0g of analytically pure niobium oxalate hydrate is added into 30-70ml of hydrochloric acid solution with the concentration of 0.1-0.5mol/l, the mixture is uniformly stirred, and then the mixture is subjected to ultrasonic dispersion to obtain transparent solution A;
2) suspending 4.3-4.7g of rape pollen in 10-50ml of 0.2-0.7mol/l hydrochloric acid solution, and uniformly stirring to obtain a mixed solution B;
3) respectively washing the mixed solution B with water and alcohol, placing the washed mixed solution B into a culture dish, adding 0.5-1g of hexadecyl trimethyl ammonium bromide into the culture dish, and heating and uniformly stirring the mixture to obtain mixed solution C;
4) adding the obtained transparent solution A and the mixed solution C into a reaction kettle, sealing, carrying out hydrothermal reaction in a homogeneous reaction instrument, naturally cooling to room temperature after the reaction is finished, and precipitating;
5) washing the precipitate obtained in the step 4) with water and alcohol respectively, placing the washed precipitate in a culture dish, transferring the culture dish into a vacuum drier, and carrying out vacuum drying at the temperature of 100 ℃ to obtain a precursor D;
6) taking the precursor D in a dry pot, raising the temperature from room temperature to 500 ℃ and 600 ℃ at the heating rate of 5 ℃/min for processing for 5h under the protection of oxygen, and then cooling along with the furnace to obtain the target product Nb2O5。
2. The preparation method of the hollowed spherical niobium oxide electrode material for the lithium ion battery according to claim 1, wherein the method comprises the following steps: the step 1) ultrasonic dispersion is carried out for 60-120 min.
3. The preparation method of the hollowed spherical niobium oxide electrode material for the lithium ion battery according to claim 1, wherein the method comprises the following steps: the filling ratio in the reaction kettle in the step 4) is 30-60%, the reaction temperature of the homogeneous phase reactor is 80-120 ℃, and the reaction time is 11-15 h.
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CN110010960A (en) * 2019-04-10 2019-07-12 陕西科技大学 A kind of indefinite form bulk Nb2O5The preparation method of anode material for lithium-ion batteries
CN111977689A (en) * 2020-07-09 2020-11-24 南阳师范学院 Niobium pentoxide microsphere with hollow structure and preparation method and application thereof

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