CN111584834B - Preparation method of metal oxide quantum dot embedded three-dimensional carbon nanomaterial - Google Patents

Preparation method of metal oxide quantum dot embedded three-dimensional carbon nanomaterial Download PDF

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CN111584834B
CN111584834B CN202010310559.XA CN202010310559A CN111584834B CN 111584834 B CN111584834 B CN 111584834B CN 202010310559 A CN202010310559 A CN 202010310559A CN 111584834 B CN111584834 B CN 111584834B
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metal oxide
quantum dot
carbon nano
oxide quantum
dimensional carbon
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CN111584834A (en
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田莎莎
李佳欣
蒋兴琳
金恺乐
尹号
曹江行
张晶晶
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China Jiliang University
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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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C01G19/02—Oxides
    • 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
    • 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
    • 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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention relates to a preparation method of a metal oxide quantum dot embedded three-dimensional carbon nano material and a preparation method thereof, which are characterized in that the metal oxide quantum dot is embedded in the inner wall of a three-dimensional carbon material by an in-situ growth method to design and synthesize a novel metal oxide quantum dot composite three-dimensional carbon nano material. Wherein the metal oxide quantum dots are: one or more of metal oxides such as tin dioxide, iron oxide, sodium oxide and the like; the three-dimensional carbon nano material is one or more of carbon nano tubes, carbon bubbles, 3D interconnected carbon nano bubbles, 3D single-connected carbon nano bubbles and the like. The tin dioxide quantum dot embedded carbon nano interconnected bubble electrode material prepared by the invention improves the conductivity of the material, relieves the volume expansion change in the charging and discharging processes, has good electrochemical performance, and can be further applied to industrial production and life.

Description

Preparation method of metal oxide quantum dot embedded three-dimensional carbon nanomaterial
Technical Field
The invention belongs to the field of lithium ion battery materials, and particularly relates to a preparation method of a metal oxide quantum dot embedded three-dimensional carbon nano material.
Background
The demand for batteries (LIBs) has increased, and researchers have conducted a great deal of research to drive the high level of sophistication for LIBsDevelopment of electrode materials. Among the various candidate materials, metal oxides such as: the tin dioxide-based material is one of potential cathode materials of the LIB due to unique characteristics, and has the advantages of low price, abundant quantity, small environmental pollution and high theoretical capacity (the theoretical capacity of the material in two conversions under the condition of taking reaction and alloying reaction into consideration is 1494 mAh g-1). Further applications of tin dioxide have been plagued by its own low electronic conductivity, solid electrolyte interfacial instability (SEI), and problems of particle agglomeration due to repeated volume changes. To solve the above problems, various research and development groups have developed many methods for improving the electrical conductivity and structural stability of metal oxides such as tin dioxide, for example, optimizing particle size, morphology, and making metal oxide/carbon hybrids.
The mechanical integrity of the electrode can be maintained by uniformly dispersing the nano metal oxide in a conductive matrix (such as graphite), so that the cycle performance and the rate capability are greatly improved. Therefore, it would be a powerful solution to have uniform metal oxide quantum dots uniformly fit on conductive carbon materials. Patent CN 103441254 a introduces a preparation method of a graphene/tin dioxide quantum dot composite electrode material for a lithium ion battery, the patent synthesizes graphene-loaded tin dioxide quantum dots under relatively mild experimental conditions by using a wet chemical method, and the preparation process adopts urea as a reducing agent to reduce graphite oxide, so that the preparation method has the advantages of simple and controllable reaction conditions and low production cost. The introduction of the graphene can improve the conductive capability of the composite material and can play an effective buffering role in volume change of tin dioxide in the charging and discharging processes. Patent CN 107055516B discloses a preparation method of a graphene/tin dioxide quantum dot composite material, which utilizes a microwave hydrothermal method to realize reduction of graphene oxide and preparation of the composite material in one step, and has the advantages of simple operation, rapid preparation and effective avoidance of secondary reduction of graphene oxide; the tin dioxide quantum dots can effectively avoid the secondary accumulation of graphene; the tin dioxide quantum dots are grown on the graphene sheet in situ, so that the electrical property of the composite material can be improved.
In the prior art, the mechanical integrity of the electrode can be kept by uniformly dispersing the nano metal oxide in a conductive matrix (such as carbon), so that the cycle performance and the rate capability are greatly improved, but only active nano particles can be scattered on the surface of the carbon to be in a naked state, and the problem of volume change is still not solved.
Disclosure of Invention
Aiming at the prior technical scheme, the invention aims to provide a preparation method for embedding metal oxide quantum dots into a three-dimensional carbon nano electrode material, overcomes the defects of the prior preparation technology, and improves the electrochemical performance of the metal oxide quantum dots embedded into the three-dimensional carbon nano electrode material. Wherein the metal oxide is: the three-dimensional carbon nano material is prepared from metal oxide materials such as tin dioxide, iron oxide, sodium oxide and the like, and the three-dimensional carbon nano material is as follows: one or more of three-dimensional carbon nanomaterials such as carbon nanotubes, carbon bubbles, 3D interconnected carbon nanobubbles, 3D single-connected carbon nanobubbles, and the like. In order to achieve the aim, the experimental scheme of the invention is that SnO is added2Quantum dots are embedded in 3D interconnected carbon nanobubbles to design and synthesize novel tin dioxide-carbon nanocomposites. Wherein the thickness of the carbon nano bubble wall is 0.8-1.2 nm, and the carbon nano bubble wall are uniformly connected with each other; the mass ratio of the carbon nanobubbles to the tin chloride is 1: 10-1: 2.
a preparation method of a tin dioxide quantum dot embedded carbon nano interconnected bubble electrode material comprises the following steps:
1) weighing a certain amount of stannic chloride, dissolving in a certain amount of distilled water, and stirring.
2) And then dispersing 0.1 g of 3D interconnected carbon nanobubbles in the solution obtained in the step 1), and carrying out ultrasonic treatment for 0.5-2 h.
3) Transferring the product obtained in the step 2) into a stainless steel autoclave lined with Teflon, and carrying out hydrothermal reaction for 12-28 h at the temperature of 80-120 ℃.
4) Cooling the product obtained in the step 3) to room temperature, centrifuging, washing and drying, wherein the temperature is controlled to be 60-80 ℃.
5) Calcining the product obtained in the step 4) in Ar atmosphere for 2-5 hours, controlling the temperature at 400-500 ℃, and raising the temperature at 2-degree Cmin-1 To obtainThe final product SnO2 quantum dot embedded carbon nano interconnected bubble electrode material.
The thickness of the carbon nano bubble wall is 0.8-1.2 nm, and the carbon nano bubble wall are uniformly connected with each other;
the tin dioxide quantum dots are uniformly distributed on the carbon nano bubble inner shell; the mass ratio of the carbon nanobubbles to the tin chloride is 1: 10-1: 2.
compared with other tin dioxide quantum dot composite carbon materials, the invention has the following advantages:
1) the tin dioxide quantum dots are mainly and uniformly distributed on the inner shell of the carbon nanobubble, and the core of the carbon nanobubble is kept hollow.
2) The carbon nano bubbles are uniformly connected with each other, and the matrix of the carbon nano bubbles is stable to adapt to mechanical stress caused by volume change of the tin dioxide quantum dots.
3) The carbon nano bubbles are uniformly connected with each other, so that a good electron transmission path is provided;
4) the tin dioxide quantum dot embedded carbon nano-interconnected bubble electrode material prepared by the invention has good electrochemical performance and the current density of 200mA g -1300 times of circulation and 1125.5 mAh g of specific capacity-1(ii) a And a current density of 1A g-11000 times of circulation and specific capacity of 560.6 mAh g-1。
5) The tin dioxide quantum dot embedded carbon material has simple process and convenient operation, and is beneficial to industrial production.
Drawings
FIG. 1 is a schematic diagram of a tin dioxide quantum dot embedded carbon nano interconnected bubble electrode material
FIG. 2 is a cycle chart of a tin dioxide quantum dot embedded carbon nano interconnected bubble electrode material
Detailed Description
In order to further understand the contents, features and effects of the present invention, the following embodiments are described in detail as follows:
example 1
A preparation method of a tin dioxide quantum dot embedded carbon nano interconnected bubble electrode material comprises the following steps:
1) weighing a certain amount of stannic chloride, dissolving in a certain amount of distilled water, and stirring.
2) And then dispersing a certain amount of 3D interconnected carbon nanobubbles in the solution obtained in the step 1), wherein the ratio of the carbon nanobubbles is 8-11%, and performing ultrasonic treatment for 0.5-2 h.
3) Transferring the product obtained in the step 2) into a stainless steel autoclave lined with Teflon, and carrying out hydrothermal reaction for 12-28 h at the temperature of 80-120 ℃.
4) Cooling the product obtained in the step 3) to room temperature, centrifuging, washing and drying, wherein the temperature is controlled to be 60-80 ℃.
5) Calcining the product obtained in the step 4) in Ar atmosphere for 2-5 hours, controlling the temperature at 400-500 ℃ and the heating rate at 2 ℃ for min-1Obtain the final product SnO2The quantum dot embedded carbon nano-interconnect bubble electrode material.
The tin dioxide quantum dot embedded carbon nano interconnected bubble electrode material; when the lithium ion battery is used for a cathode of a lithium ion battery; the electrochemical performance is general, 200mAh g-1Under the current density, after 300 times of electric circulation, the charge-discharge capacity of the material is more than 187.8 mAh g-1。
Example 2
A preparation method of a tin dioxide quantum dot embedded carbon nano interconnected bubble electrode material comprises the following steps:
1) weighing a certain amount of stannic chloride, dissolving in a certain amount of distilled water, and stirring.
2) And then dispersing a certain amount of 3D interconnected carbon nanobubbles in the solution obtained in the step 1), wherein the proportion of the carbon nanobubbles is 18-21%, and performing ultrasonic treatment for 0.5-2 h.
3) Transferring the product obtained in the step 2) into a stainless steel autoclave lined with Teflon, and carrying out hydrothermal reaction for 12-28 h at the temperature of 80-120 ℃.
4) Cooling the product obtained in the step 3) to room temperature, centrifuging, washing and drying, wherein the temperature is controlled to be 60-80 ℃.
5) Calcining the product obtained in the step 4) in Ar atmosphere for 2-5 hours, controlling the temperature at 400-500 ℃ and the heating rate at 2 ℃ for min-1Obtain the final product SnO2The quantum dot embedded carbon nano-interconnect bubble electrode material.
The tin dioxide quantum dot embedded carbon nano interconnected bubble electrode material; when the lithium ion battery is used for a cathode of a lithium ion battery; good electrochemical performance, 200mAh g-1Under the current density, after 300 times of electric circulation, the charge-discharge capacity of the material is more than 1125.5 mAh g-1。
Example 3
1) A preparation method of a tin dioxide quantum dot embedded carbon nano interconnected bubble electrode material comprises the following steps:
2) weighing a certain amount of stannic chloride, dissolving in a certain amount of distilled water, and stirring.
3) And then dispersing a certain amount of 3D interconnected carbon nanobubbles in the solution obtained in the step 1), wherein the ratio of the carbon nanobubbles is 37-41%, and performing ultrasonic treatment for 0.5-2 h.
4) Transferring the product obtained in the step 2) into a stainless steel autoclave lined with Teflon, and carrying out hydrothermal reaction for 12-28 h at the temperature of 80-120 ℃.
5) Cooling the product obtained in the step 3) to room temperature, centrifuging, washing and drying, wherein the temperature is controlled to be 60-80 ℃.
6) Calcining the product obtained in the step 4) in Ar atmosphere for 2-5 hours, controlling the temperature at 400-500 ℃ and the heating rate at 2 ℃ for min-1Obtain the final product SnO2The quantum dot embedded carbon nano-interconnect bubble electrode material.
The tin dioxide quantum dot embedded carbon nano interconnected bubble electrode material; when the lithium ion battery is used for a cathode of a lithium ion battery; good electrochemical performance, 200mAh g-1Under the current density, after 300 times of electric circulation, the charge-discharge capacity of the material is more than 771.1 mAh g-1。
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (3)

1. A preparation method of a metal oxide quantum dot embedded three-dimensional carbon nanomaterial is characterized in that the metal oxide quantum dot is embedded in the three-dimensional carbon nanomaterial to design and synthesize a metal oxide quantum dot-carbon nanocomposite electrode material; the metal oxide quantum dots are: tin dioxide quantum dots; the three-dimensional carbon nano material is 3D interconnected carbon nanobubbles; the tin dioxide quantum dots are uniformly distributed on the inner shell of the 3D interconnected carbon nanobubbles, and the core of the 3D interconnected carbon nanobubbles is kept hollow;
the preparation method comprises the following steps:
1) weighing a certain amount of stannic chloride, dissolving in a certain amount of distilled water, and stirring;
2) then dispersing a certain amount of 3D interconnected carbon nano bubbles in the solution obtained in the step 1), wherein the 3D interconnected carbon nano bubbles account for 18-21%, and performing ultrasonic treatment for 0.5-2 h;
3) transferring the product obtained in the step 2) into a stainless steel autoclave lined with Teflon, and carrying out hydrothermal reaction for 12-28 h at the temperature of 80-120 ℃;
4) cooling the product obtained in the step 3) to room temperature, centrifuging, washing and drying, wherein the drying temperature is controlled to be 60-80 ℃;
5) calcining the product obtained in the step 4) in Ar atmosphere for 2-5 h, controlling the temperature to be 400-500 ℃, and raising the temperature at the rate of 2 ℃ for min-1And finally, embedding the metal oxide quantum dots into the 3D interconnected carbon nano bubble electrode material.
2. The method for preparing the metal oxide quantum dot embedded three-dimensional carbon nanomaterial according to claim 1, wherein the thickness of the 3D interconnected carbon nanobubble wall in the three-dimensional carbon nanomaterial is 0.8-1.2 nm, and the three-dimensional carbon nanomaterial is uniformly connected with each other.
3. The method for preparing the metal oxide quantum dot embedded three-dimensional carbon nanomaterial according to claim 1, wherein the mass ratio of the three-dimensional carbon nanomaterial to the metal oxide is 1: 1-1: 3.
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