CN111675241A - Preparation method of tungsten dioxide nanowire array/zinc stannate nanoribbon cathode material, product and application - Google Patents

Preparation method of tungsten dioxide nanowire array/zinc stannate nanoribbon cathode material, product and application Download PDF

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CN111675241A
CN111675241A CN202010523476.9A CN202010523476A CN111675241A CN 111675241 A CN111675241 A CN 111675241A CN 202010523476 A CN202010523476 A CN 202010523476A CN 111675241 A CN111675241 A CN 111675241A
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zinc stannate
nanobelt
nanowire array
dioxide nanowire
tungsten dioxide
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崔大祥
吴晓燕
林琳
王敬锋
王岩岩
徐少洪
陈超
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00—Compounds of tungsten
    • C01G41/02—Oxides; Hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
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    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • H—ELECTRICITY
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    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
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    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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Abstract

The invention provides a preparation method of a tungsten dioxide nanowire array/zinc stannate nanobelt cathode material and a product and application thereof, wherein zinc dioxide, stannic oxide and alkali metal alkali solution are mixed, magnetically stirred, transferred into a hydrothermal kettle for reaction, cleaned, dried and calcined to obtain a zinc stannate nanobelt; mixing sodium tungstate and dilute acid to obtain a precursor solution, putting the zinc stannate nanobelt serving as a substrate into the precursor solution, transferring the precursor solution into a reaction kettle for reaction, and then cleaning and drying the precursor solution to obtain the tungsten dioxide nanowire array/the zinc stannate nanobelt. The preparation process is relatively simple and easy to operate. The titanium dioxide nanowire array and the zinc stannate nanobelt prepared by the method have larger specific surface area and conductivity, and are beneficial to further improving the electrochemical performance of the material. The tungsten dioxide nanowire array/zinc stannate nanobelt of the product has the specific first discharge capacity of 1580 mAh/g and higher specific discharge capacity.

Description

Preparation method of tungsten dioxide nanowire array/zinc stannate nanoribbon cathode material, product and application
Technical Field
The invention relates to a preparation method of a lithium battery cathode material, in particular to a preparation method of a tungsten dioxide nanowire array/zinc stannate nanobelt cathode material, and a product and application thereof.
Background
With the development of society, lithium ion batteries are receiving much attention. The lithium ion battery is the most ideal rechargeable battery in the world at present, and has the advantages of high energy density, long cycle life, no memory effect, small pollution and the like. With the progress of technology, lithium ion batteries are widely applied to the fields of electric automobiles, aerospace, biomedicine and the like, so that the research and development of lithium ion batteries for power and related materials have great significance. For power lithium ion batteries, the key is to increase the power density and energy density, and the improvement of the power density and energy density is fundamentally the improvement of electrode materials, particularly negative electrode materials.
Since the early 90 s of the last century, the japanese scientists developed carbon materials with layered structures, which were the first materials studied by people and applied to the commercialization of lithium ion batteries, and still remain one of the major points of attention and research, but carbon negative electrode materials have some defects: when the battery is formed, the electrolyte reacts with the electrolyte to form an SEI film, so that the electrolyte is consumed and the first coulombic efficiency is low; when the battery is overcharged, metal lithium may be precipitated on the surface of the carbon electrode to form lithium dendrite to cause short circuit, so that the temperature is increased and the battery explodes; in addition, the diffusion coefficient of lithium ions in the carbon material is small, so that the battery cannot realize large-current charging and discharging, and the application range of the lithium ion battery is limited.
Zinc stannate (Zn)2SnO4) Is a spinel-structured composite oxide which can be used as a lithium ion battery cathode material at present, but the zinc stannate has insufficient electrochemical performance and needs to have higher Li through conversion and alloying reactions+A storage capacity. The material is considered to be a promising lithium ion battery cathode material.
Disclosure of Invention
In order to overcome the defect of poor electrochemical performance of zinc stannate, the invention aims to: provides a preparation method of a tungsten dioxide nanowire array/zinc stannate nanobelt anode material.
Yet another object of the present invention is to: provides a tungsten dioxide nanowire array/zinc stannate nanobelt anode material product obtained by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of a tungsten dioxide nanowire array/zinc stannate nanobelt anode material comprises the following steps:
(1) preparing a zinc stannate nanobelt: mixing zinc dioxide, tin dioxide and alkali metal alkali solution in a molar ratio of 2:1:300, and magnetically stirring for 1-2 hours until the solution is clear; transferring the mixture into a hydrothermal kettle to react for 24-36 h at 160-180 ℃, washing the mixture for 3-5 times by using dilute acid, then drying the mixture in vacuum, and then calcining the mixture in a muffle furnace for 2-4 h at 450-500 ℃ to obtain a zinc stannate nanobelt;
(2) mixing sodium tungstate and dilute acid to obtain a precursor solution with the W concentration of 0.01-0.05 mol/L;
(3) and (3) putting the zinc stannate nanobelt serving as a substrate into the precursor solution, then transferring the zinc stannate nanobelt into a reaction kettle for reaction at the temperature of 140-160 ℃ for 3-6 hours, and cleaning and drying to finally obtain the tungsten dioxide nanowire array/the zinc stannate nanobelt.
The invention provides a preparation method of a tungsten dioxide nanowire array/zinc stannate nanobelt cathode material, wherein the tungsten dioxide nanowire array and zinc stannate nanobelt composite material has larger specific surface area and conductivity, and is beneficial to further improving the electrochemical performance of the material. The preparation process is relatively simple and easy to operate.
On the basis of the scheme, the alkali metal base is one or the combination of sodium hydroxide or potassium hydroxide.
Preferably, the dilute acid is one or a combination of dilute hydrochloric acid and dilute nitric acid.
The invention also provides a tungsten dioxide nanowire array/zinc stannate nanobelt anode material which is prepared according to any one of the methods.
The invention also provides application of the tungsten dioxide nanowire array/zinc stannate nanobelt cathode material in a lithium ion battery.
The invention provides a preparation method of a tungsten dioxide nanowire array/zinc stannate nanobelt anode material, which is relatively simple in process and easy to operate. The prepared tungsten dioxide nanowire array and zinc stannate nanobelt have larger specific surface area and conductivity, and are beneficial to further improving the electrochemical performance of the material. The product of the invention can reach 1580 mAh/g as a negative electrode material, and has higher specific discharge capacity.
Drawings
FIG. 1 is a graph of the first discharge performance of the tungsten dioxide nanowire array/zinc stannate nanoribbon of example 1;
FIG. 2 is a graph of the first discharge performance of the tungsten dioxide nanowire array/zinc stannate nanoribbon of example 2;
FIG. 3 is a graph of the first discharge performance of the tungsten dioxide nanowire arrays/zinc stannate nanoribbons of example 3.
Detailed Description
The present invention is described in detail by the following specific examples, but the scope of the present invention is not limited to these examples.
Example 1
A tungsten dioxide nanowire array/zinc stannate nanobelt anode material is prepared by the following steps:
(1) preparing a zinc stannate nanobelt: mixing zinc dioxide, tin dioxide and sodium hydroxide solution with a molar ratio of 2:1:300, and magnetically stirring for 1h until the solution is clear; transferring the mixture into a hydrothermal kettle to react for 24 hours at 160 ℃, washing the mixture for 3 times by using dilute hydrochloric acid, drying the mixture in vacuum, and then calcining the mixture in a muffle furnace for 2 hours at 500 ℃ to obtain a zinc stannate nanobelt;
(2) mixing sodium tungstate and dilute hydrochloric acid to obtain a precursor solution with the tungsten (W) concentration of 0.01 mol/L;
(3) and putting the zinc stannate nanobelt serving as a substrate into the precursor solution, transferring the precursor solution into a reaction kettle for reaction at 140 ℃ for 6 hours, and cleaning and drying to finally obtain the tungsten dioxide nanowire array/the zinc stannate nanobelt.
FIG. 1 is a graph showing the first discharge performance of the tungsten dioxide nanowire array/zinc stannate nanoribbon product of this example; the first discharge specific capacity is 1580 mAh/g, and the discharge specific capacity is higher.
Example 2
The tungsten dioxide nanowire array/zinc stannate nanobelt anode material is prepared by the following steps, similar to the embodiment:
(1) preparing a zinc stannate nanobelt: mixing zinc dioxide, tin dioxide and sodium hydroxide solution according to the molar ratio of 2:1:300, and magnetically stirring for 2 hours until the solution is clear; transferring the mixture into a hydrothermal kettle to react for 24 hours at 180 ℃, washing the mixture for 5 times by using dilute nitric acid, drying the mixture in vacuum, and calcining the mixture in a muffle furnace for 4 hours at 450 ℃ to obtain a zinc stannate nanobelt;
(2) mixing sodium tungstate and dilute nitric acid to obtain a precursor solution, wherein the concentration of W is controlled to be 0.03 mol/L;
(3) and putting the zinc stannate nanobelt serving as a substrate into the precursor solution, transferring the zinc stannate nanobelt into a reaction kettle to react for 3 hours at 160 ℃, and finally obtaining the tungsten dioxide nanowire array/the zinc stannate nanobelt after cleaning and drying.
FIG. 2 is a graph of the first discharge performance of the tungsten dioxide nanowire array/zinc stannate nanoribbon of this embodiment; the first discharge specific capacity is 1370 mAh/g.
Example 3
The tungsten dioxide nanowire array/zinc stannate nanobelt anode material is prepared by the following steps, similar to the embodiment:
(1) preparing a zinc stannate nanobelt: mixing zinc dioxide, tin dioxide and potassium hydroxide alkali solution according to the molar ratio of 2:1:300, and magnetically stirring for 2 hours until the solution is clear; transferring the mixture into a hydrothermal kettle to react for 24 hours at 180 ℃, washing the mixture for 3 times by using dilute nitric acid, drying the mixture in vacuum, and calcining the mixture in a muffle furnace for 4 hours at 500 ℃ to obtain a zinc stannate nanobelt;
(2) mixing sodium tungstate and dilute nitric acid to obtain a precursor solution, wherein the concentration of W is controlled to be 0.05 mol/L;
(3) and putting the zinc stannate nanobelt serving as a substrate into the precursor solution, then transferring the zinc stannate nanobelt into a reaction kettle to react for 3 hours at 160 ℃, and finally obtaining the tungsten dioxide nanowire array/the zinc stannate nanobelt after cleaning and drying.
FIG. 3 is a graph of the first discharge performance of tungsten dioxide nanowire arrays/zinc stannate nanoribbons; the first discharge specific capacity is 1500 mAh/g.

Claims (5)

1. A preparation method of a tungsten dioxide nanowire array/zinc stannate nanobelt cathode material is characterized by comprising the following steps:
(1) preparing a zinc stannate nanobelt: mixing zinc dioxide, tin dioxide and alkali metal alkali solution in a molar ratio of 2:1:300, and magnetically stirring for 1-2 hours until the solution is clear; transferring the mixture into a hydrothermal kettle, reacting for 24-36 h at 160-180 ℃, washing for 3-5 times by using dilute acid, drying in vacuum, and calcining for 2-4 h in a muffle furnace at 450-500 ℃ to obtain a zinc stannate nanobelt;
(2) mixing sodium tungstate and dilute acid to obtain a precursor solution with the tungsten (W) concentration of 0.01-0.05 mol/L;
(3) and (3) putting the zinc stannate nanobelt serving as a substrate into the precursor solution, transferring the zinc stannate nanobelt into a reaction kettle to react for 3-6 hours at the temperature of 140-160 ℃, and cleaning and drying to obtain the tungsten dioxide nanowire array/zinc stannate nanobelt.
2. The method for preparing the tungsten dioxide nanowire array/zinc stannate nanoribbon anode material of claim 1, wherein in the step (1), the alkali metal base is one or a combination of sodium hydroxide and potassium hydroxide.
3. The method for preparing the tungsten dioxide nanowire array/zinc stannate nanoribbon anode material according to claim 1, wherein the dilute acid is one or a combination of dilute hydrochloric acid and dilute nitric acid.
4. A tungsten dioxide nanowire array/zinc stannate nanoribbon negative electrode material, which is characterized by being prepared according to any one of the methods of claims 1-3.
5. The use of the tungsten dioxide nanowire array/zinc stannate nanoribbon anode material of claim 4 in a lithium ion battery.
CN202010523476.9A 2020-06-10 2020-06-10 Preparation method of tungsten dioxide nanowire array/zinc stannate nanoribbon cathode material, product and application Pending CN111675241A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101798117A (en) * 2010-03-24 2010-08-11 桂林理工大学 Method for preparing highly ordered tungsten trioxide nano-rod
CN103395842A (en) * 2013-07-30 2013-11-20 浙江大学 Tungsten trioxide nanometer array electrochromic film and preparation method thereof
CN104891557A (en) * 2015-05-29 2015-09-09 吉林大学 Tin dioxide nanoflower with hollow structure and preparation method of tin dioxide nanoflower
US20160041116A1 (en) * 2014-08-06 2016-02-11 Korea Advanced Institute Of Science And Technology Composite metal oxide materials including polycrystalline nanofibers, microparticles, and nanoparticles, gas sensors using the same as a sensing material thereof, and manufacturing methods thereof
CN110408953A (en) * 2019-08-13 2019-11-05 哈尔滨理工大学 A kind of porous core-shell nano line flexible array electrode of phosphorus doping tungsten sulfide@tungsten oxide and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101798117A (en) * 2010-03-24 2010-08-11 桂林理工大学 Method for preparing highly ordered tungsten trioxide nano-rod
CN103395842A (en) * 2013-07-30 2013-11-20 浙江大学 Tungsten trioxide nanometer array electrochromic film and preparation method thereof
US20160041116A1 (en) * 2014-08-06 2016-02-11 Korea Advanced Institute Of Science And Technology Composite metal oxide materials including polycrystalline nanofibers, microparticles, and nanoparticles, gas sensors using the same as a sensing material thereof, and manufacturing methods thereof
CN104891557A (en) * 2015-05-29 2015-09-09 吉林大学 Tin dioxide nanoflower with hollow structure and preparation method of tin dioxide nanoflower
CN110408953A (en) * 2019-08-13 2019-11-05 哈尔滨理工大学 A kind of porous core-shell nano line flexible array electrode of phosphorus doping tungsten sulfide@tungsten oxide and preparation method thereof

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* Cited by examiner, † Cited by third party
Title
马世昌: "《基础化学反应》", 31 January 2003, 陕西科学技术出版社 *

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