CN113428890A - Multilevel-structure CuS hollow sphere, preparation method and application thereof - Google Patents

Multilevel-structure CuS hollow sphere, preparation method and application thereof Download PDF

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CN113428890A
CN113428890A CN202110910606.9A CN202110910606A CN113428890A CN 113428890 A CN113428890 A CN 113428890A CN 202110910606 A CN202110910606 A CN 202110910606A CN 113428890 A CN113428890 A CN 113428890A
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cus
hollow sphere
multilevel structure
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CN113428890B (en
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张利锋
胡越
白嘉玺
李帅
阮欢
刘毅
郭守武
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Shaanxi University of Science and Technology
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    • C01G3/00—Compounds of copper
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    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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    • H01M4/5815—Sulfides
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    • C01P2004/32—Spheres
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Abstract

The invention provides a CuS hollow sphere with a multilevel structure, a preparation method and application thereof, and belongs to the field of micro-nano material synthesis. The invention takes a copper source with lower cost as a sulfur source as a reaction raw material, and prepares the CuS nano material by adopting a simple oil bath method and adjusting process parameters. The invention has the advantages of low price of raw materials, simple preparation process, lower preparation cost, suitability for industrial production and wide application prospect. According to the preparation method disclosed by the invention, the size of the CuS nano material can be regulated and controlled by changing reaction parameters, and the prepared CuS has a distinct shape characteristic, has a unique hollow spherical shape with a multi-stage structure, is used as a negative electrode material of a sodium-ion battery, and has a good electrochemical performance.

Description

Multilevel-structure CuS hollow sphere, preparation method and application thereof
Technical Field
The invention belongs to the field of micro-nano material synthesis, and particularly relates to a CuS hollow sphere with a multilevel structure, a preparation method and application thereof.
Background
CuS is an important transition metal sulfide, has excellent photoelectric properties, and is an important P-type semiconductor material. The CuS nano material is widely applied to the fields of photoelectric conversion switches, solar cells, gas sensors, light emitting diodes, photocatalysts, electrochemical cells, optical recording materials and the like.
At present, researchers adopt various means such as a hydrothermal method, a template method, a microwave method and the like to prepare various CuS nano materials such as nano particles, nano wires, nano rods, nano sheets, hollow spheres and the like. Due to the special structure of the hollow sphere, the CuS hollow sphere has more researches in recent years, and is synthesized by adopting different templates. For example, Liu et al prepared CuS hollow semiconductor spheres by a one-step solvothermal method using H2S foam as a template (Journal of Crystal Growth,2009,311(3): 500-. In addition, sea and the like adopt a microwave radiation method to prepare a CuS submicron hollow sphere structure with the particle size of about 400nm (journal of radiation research and radiation technology 2010). Huang et al prepared CuS hollow spheres with latex particles of styrene-acrylic acid copolymer as a template (Ceramics International,2009,35(2): 905-. Chinese patent CN200710302191.7 uses polymer hollow sphere as template to combine with sol-gel, settling reaction, and redox process, and prepares composite hollow sphere by forced interface method or surface settling method, and removes the template polymer by high temperature sintering or selective extraction of solvent to obtain inorganic, metal, and organic hollow sphere. The template agent is usually added in the process of preparing the hollow sphere structure of the CuS nano material disclosed above, and the CuS nano material needs to be removed by methods such as etching, calcining and the like at the later stage, so that the preparation process is relatively complex.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a CuS hollow sphere with a multilevel structure, a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a preparation method of a CuS hollow sphere with a multilevel structure comprises the following steps:
1) dissolving a copper source in 1, 2-propylene glycol according to the concentration of 0.01-0.04 mol/L to prepare a solution A;
2) dissolving a sulfur source in deionized water according to the concentration of 0.01-0.02 mol/L to prepare a solution B;
3) mixing the solution A and the solution B according to a volume ratio of 1: (0.2-1) mixing;
4) and (3) reacting the mixed solution at 30-60 ℃ for 10-14 hours, and after the reaction is finished, washing and drying to obtain the CuS hollow sphere with the multilevel structure.
Further, in step 1), the copper source is copper trifluoromethanesulfonate, acetylacetone or copper molybdate.
Further, in step 1), the sulfur source is thiosemicarbazide, ammonium thiosulfate or L-methionine.
Furthermore, the washing times are 3-6 times, the vacuum drying temperature is 60-80 ℃, and the drying time is 8-11 hours.
The invention discloses a CuS hollow sphere with a multilevel structure, which is prepared according to the preparation method provided by the invention.
Furthermore, the diameter is 270-300 nm.
Furthermore, the nano-material is assembled by a one-dimensional nano-rod and a two-dimensional nano-sheet.
The invention relates to application of a CuS hollow sphere with a multilevel structure as a negative electrode material of a sodium-ion battery.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the CuS hollow sphere sodium ion battery cathode material with the multilevel structure has the advantages of common and easily-obtained raw materials, simple equipment, simple and convenient preparation process and strong repeatability, and is favorable for industrial batch production. According to the preparation method, the size of the CuS hollow sphere can be regulated and controlled by changing reaction parameters, and a product with good electrochemical performance can be prepared according to needs.
The CuS nano material prepared by the invention is obviously different from a common CuS material in structure, firstly, the CuS one-dimensional nano rod and the two-dimensional nano sheet are mutually interwoven to form a primary structure of the CuS; and secondly, the CuS nanosheets and the rods are jointly self-assembled into a porous CuS hollow sphere to form a CuS secondary structure.
When the CuS hollow sphere with the multilevel structure is used as a cathode material of a sodium ion battery, the nanosheets can provide more active sites in the unique multilevel structure of the CuS, the nanorods can be used as a framework to stabilize the structure of the CuS, and the hollow part can buffer the volume change of the CuS in the charging and discharging process.
Drawings
FIG. 1 is an XRD pattern of a CuS hollow sphere prepared in example 1;
FIG. 2 is a scanning electron micrograph of a CuS hollow sphere prepared in example 1;
FIG. 3 is a transmission electron micrograph of a CuS hollow sphere prepared in example 1;
FIG. 4 is a cycle chart of the CuS hollow spheres prepared in example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
example 1
1) Dissolving 0.01mol/L copper trifluoromethanesulfonate in 1, 2-propylene glycol to prepare a solution A;
2) dissolving 0.01mol/L thiosemicarbazide in deionized water to prepare a solution B;
3) and (3) mixing the solution A and the solution B according to the volume ratio of 1: 0.2 mixing;
4) and (3) reacting the mixed solution at 60 ℃ for 10 hours, washing the mixed solution for 3 times by using deionized water and ethanol after the reaction is finished, and drying the mixed solution in vacuum at 60 ℃ for 11 hours to obtain the CuS hollow sphere with the multilevel structure.
Referring to fig. 1, fig. 1 is an XRD chart of the CuS micro-nano material prepared by the present invention, and from fig. 1, it can be determined that the composition of the CuS hollow sphere phase has high purity.
Referring to fig. 2, fig. 2 is a scanning electron microscope image of the product of example 1, wherein the prepared CuS hollow sphere has a distinct appearance, is in a regular nano-sphere shape, and has a diameter of about 270 to 300 nm.
Referring to fig. 1, fig. 3 is a transmission electron microscope image of the product, from which it can be seen that the CuS one-dimensional nanorod and the two-dimensional nanosheet self-assemble into a unique nano-scale multilevel structure hollow sphere.
Referring to fig. 4, fig. 4 shows a cycle chart of the CuS hollow sphere as a negative electrode material of a sodium ion battery, wherein, at a current density of 10A/g, the specific discharge capacity after 100 cycles is 309mAh/g, and the coulomb efficiency is close to 99%.
Example 2
1) 0.04mol/L of acetylacetone is dissolved in 1, 2-propylene glycol to prepare a solution A;
2) dissolving 0.02mol/L ammonium thiosulfate in deionized water to prepare a solution B;
3) and (3) mixing the solution A and the solution B according to the volume ratio of 1: 1, mixing;
4) and (3) reacting the mixed solution at 30 ℃ for 14 hours, washing the mixed solution for 6 times by using deionized water and ethanol after the reaction is finished, and drying the washed mixed solution for 8 hours in vacuum at 80 ℃ to obtain the CuS hollow sphere with the multilevel structure.
Example 3
1) Dissolving 0.02mol/L copper molybdate in 1, 2-propylene glycol to prepare a solution A;
2) dissolving 0.02 mol/L-methionine in deionized water to prepare a solution B;
3) and (3) mixing the solution A and the solution B according to the volume ratio of 1: 0.4 mixing;
4) and (3) reacting the mixed solution at 50 ℃ for 12 hours, washing the mixed solution for 5 times by using deionized water and ethanol after the reaction is finished, and performing vacuum drying at 70 ℃ for 9 hours to obtain the CuS hollow sphere with the multilevel structure.
Example 4
1) Dissolving 0.03mol/L copper trifluoromethanesulfonate in 1, 2-propylene glycol to prepare a solution A;
2) dissolving 0.01mol/L thiosemicarbazide in deionized water to prepare a solution B;
3) and (3) mixing the solution A and the solution B according to the volume ratio of 1: 0.6 mixing;
4) and (3) reacting the mixed solution at 60 ℃ for 9 hours, washing the mixed solution for 4 times by using deionized water and ethanol after the reaction is finished, and performing vacuum drying at 60 ℃ for 10 hours to obtain the CuS hollow sphere with the multilevel structure.
The invention completes the preparation of the CuS hollow sphere by using cheap and easily obtained raw materials and simple and efficient preparation conditions, obtains a unique hollow spherical shape with a multilevel structure, and has better electrochemical performance when being used as a cathode material of a sodium-ion battery.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (8)

1. A preparation method of a CuS hollow sphere with a multilevel structure is characterized by comprising the following steps:
1) dissolving a copper source in 1, 2-propylene glycol according to the concentration of 0.01-0.04 mol/L to prepare a solution A;
2) dissolving a sulfur source in deionized water according to the concentration of 0.01-0.02 mol/L to prepare a solution B;
3) mixing the solution A and the solution B according to a volume ratio of 1: (0.2-1) mixing;
4) and (3) reacting the mixed solution at 30-60 ℃ for 10-14 hours, and after the reaction is finished, washing and drying to obtain the CuS hollow sphere with the multilevel structure.
2. The method for preparing the CuS hollow sphere with the multilevel structure according to claim 1, wherein in the step 1), the copper source is copper trifluoromethanesulfonate, acetylacetone or copper molybdate.
3. The method for preparing a multilevel structure CuS hollow sphere according to claim 1, wherein in step 1), the sulfur source is thiosemicarbazide, ammonium thiosulfate or L-methionine.
4. The method for preparing the CuS hollow sphere with the multilevel structure according to claim 1, wherein in the step 4), the washing times are 3-6 times, the vacuum drying temperature is 60-80 ℃, and the drying time is 8-11 hours.
5. A CuS hollow sphere with a multilevel structure, which is prepared according to the preparation method of any one of claims 1 to 4.
6. The CuS hollow sphere with the multilevel structure according to claim 5, wherein the diameter is 270-300 nm.
7. The CuS hollow sphere with the multilevel structure according to claim 5, which is assembled by one-dimensional nanorods and two-dimensional nanosheets.
8. The application of the CuS hollow sphere with the multilevel structure of claim 5 as a negative electrode material of a sodium-ion battery.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114229884A (en) * 2021-10-28 2022-03-25 广东邦普循环科技有限公司 Metal sulfide sodium ion battery cathode material and preparation method thereof
CN114804187A (en) * 2022-03-22 2022-07-29 邯郸学院 Preparation method of open-ended copper sulfide hollow nanospheres

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CN103663540A (en) * 2013-12-07 2014-03-26 合肥学院 Simple preparation method of hollow spherical CuS nanometer material
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CN103663540A (en) * 2013-12-07 2014-03-26 合肥学院 Simple preparation method of hollow spherical CuS nanometer material
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114229884A (en) * 2021-10-28 2022-03-25 广东邦普循环科技有限公司 Metal sulfide sodium ion battery cathode material and preparation method thereof
WO2023071394A1 (en) * 2021-10-28 2023-05-04 广东邦普循环科技有限公司 Metal sulfide negative electrode material for sodium ion battery, and preparation method therefor
GB2616232A (en) * 2021-10-28 2023-08-30 Guangdong Brunp Recycling Technology Co Ltd Metal sulfide negative electrode material for sodium ion battery, and preparation method therefor
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CN114804187A (en) * 2022-03-22 2022-07-29 邯郸学院 Preparation method of open-ended copper sulfide hollow nanospheres
CN114804187B (en) * 2022-03-22 2023-10-27 邯郸学院 Preparation method of open copper sulfide hollow nanospheres

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