CN114122388B - CuSe nano material for sodium ion battery and preparation method thereof - Google Patents
CuSe nano material for sodium ion battery and preparation method thereof Download PDFInfo
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- CN114122388B CN114122388B CN202111391001.XA CN202111391001A CN114122388B CN 114122388 B CN114122388 B CN 114122388B CN 202111391001 A CN202111391001 A CN 202111391001A CN 114122388 B CN114122388 B CN 114122388B
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- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910001415 sodium ion Inorganic materials 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 6
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 9
- 239000002135 nanosheet Substances 0.000 abstract description 7
- 239000007772 electrode material Substances 0.000 abstract description 4
- 239000010949 copper Substances 0.000 abstract description 3
- 239000011669 selenium Substances 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract 1
- 239000008139 complexing agent Substances 0.000 abstract 1
- 229910052802 copper Inorganic materials 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 229910052711 selenium Inorganic materials 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002064 nanoplatelet Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- BVTBRVFYZUCAKH-UHFFFAOYSA-L disodium selenite Chemical compound [Na+].[Na+].[O-][Se]([O-])=O BVTBRVFYZUCAKH-UHFFFAOYSA-L 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- VVNXEADCOVSAER-UHFFFAOYSA-N lithium sodium Chemical compound [Li].[Na] VVNXEADCOVSAER-UHFFFAOYSA-N 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- IRPLSAGFWHCJIQ-UHFFFAOYSA-N selanylidenecopper Chemical compound [Se]=[Cu] IRPLSAGFWHCJIQ-UHFFFAOYSA-N 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 229960001471 sodium selenite Drugs 0.000 description 1
- 239000011781 sodium selenite Substances 0.000 description 1
- 235000015921 sodium selenite Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal selenide Chemical class 0.000 description 1
Classifications
-
- 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
- H01M4/58—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
-
- 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
-
- 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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
A CuSe nanometer material for sodium ion battery and a preparation method thereof belong to the field of sodium ion battery, and the nanometer material is of a sheet nanometer structure. The CuSe nano material adopts a one-step hydrothermal synthesis method, se powder is used as a selenium source, CTAB is used as a complexing agent, and Cu (NO) 3 ) 2 ·3H 2 O is a copper source, and the CuSe nano sheet is hydrothermally synthesized. The prepared CuSe has the characteristics of high structural purity, uniform morphology and different particle sizes. The initial specific capacity of the sodium ion battery can reach 425.2mAh/g, the initial coulomb efficiency is 96.9%, and the capacity of the electrode after 120 times of circulation is 335.1mAh/g. The CuSe nano electrode material prepared by the method has the characteristics of high specific capacitance, good cycle performance, simple preparation method, low cost and the like.
Description
Technical Field
A preparation method of a CuSe nanometer material for a sodium ion battery belongs to the field of sodium ion batteries.
Technical Field
In recent years, with the increasing prominence of the problems of traditional energy sources, the national carbon-neutral-carbon peak policy comes out, and new energy sources such as solar energy, wind energy, tidal energy and the like become hot research directions. The market application of new energy sources is greatly resisted due to the limitation of weather and regions, and the converted electric energy can be stored along with the addition of a chemical power source and then is transmitted to users by using a power grid. Particularly, the appearance of secondary batteries greatly promotes the application of new energy. Although lithium batteries are mainly used at the present stage, the lithium batteries are limited in large-scale energy storage application due to the influence of lithium resource reserves, distribution and price. In contrast, sodium resources are high in storage quantity, uniform in distribution and relatively low in price, sodium and lithium belong to the same group of elements, and the sodium and lithium are similar in property, so that the sodium-lithium composite material is more suitable for large-scale energy storage application. Therefore, the research and development of sodium ion batteries have become one of the directions of hot spot research in the field of secondary batteries.
Development of electrode materials, particularly research on high-performance anode materials, is one of key factors for development and application of sodium ion batteries. The transition metal selenide has been receiving a great deal of attention because of its high theoretical specific capacity, excellent cycle stability, and other properties. Among them, copper selenide has the advantages of higher theoretical specific capacity, high electron conductivity and the like, and is widely reported. The existing literature for preparing the flaky CuSe nano material mainly adopts hydrazine hydrate, sodium borohydride and other explosion-prone dangerous control materials as Se reducing agents or adopts sodium selenite and the like with relatively high price as Se sources. In addition, the existing preparation methods mainly comprise a high-temperature selenizing method, a multi-step liquid phase method, a microwave auxiliary method and the like, the preparation process is complicated, and therefore mixed phases in the product can be possibly caused, in addition, some preparation methods have certain requirements on equipment, so that the cost is high, and the preparation method is not beneficial to actual industrialized scale preparation.
Disclosure of Invention
The invention provides a method with low raw material price, simple preparation process, short period, mild reaction condition and safe and simple operation, and the prepared nano flaky CuSe material has high purity and good electrochemical performance when being used as a negative electrode of a sodium ion battery.
The invention provides a preparation method of a CuSe nano sheet material for a sodium ion battery, which comprises the following steps:
a) Adding deionized water and sodium hydroxide into a 100mL reaction kettle, stirring at room temperature for dissolution, and then adding selenium powder;
b) Stirring at room temperature for 10min, and adding cetyl trimethyl ammonium bromide and copper nitrate trihydrate;
c) Stirring for 10min at room temperature, placing the reaction kettle in a baking oven for hydrothermal synthesis reaction, and carrying out centrifugal water washing and drying treatment;
d) The CuSe nano sheet material is used as an electrode material to be applied to a sodium ion battery.
The addition amounts of deionized water, sodium hydroxide and selenium powder in the step a) are 45.0mL, 208.3mmol and 3.2mmol respectively;
the addition amounts of cetyl trimethyl ammonium bromide and copper nitrate trihydrate in the step b) are 2.1mmol and 2.0mmol respectively;
the temperature of the hydrothermal synthesis reaction in the step c) is 140 ℃, and the reaction time is 1-2.0 h.
In the step d), in the sodium ion battery cycle performance test, the initial specific capacity can reach 425.2mAh/g, the initial coulomb efficiency is 96.9%, and the capacity of the electrode still reaches 335.1mAh/g after 120 cycles.
Compared with other methods for preparing the flaky CuSe, the method has the advantages that the preparation process is greatly simplified, the raw materials which are cheap and easy to obtain are adopted, the preparation conditions are mild and safe, the method is suitable for large-scale production, the production cost is reduced, and the production period is shortened; more importantly, the prepared pure-phase CuSe nano sheet has higher specific capacity and cycle performance when being used for sodium ion batteries.
A Bruker Advance D8X-ray powder diffractometer (Cu ka radiation,2 θ=10 to 80°) the structure of the prepared material was determined. The surface morphology of the prepared material was observed using a Hitachi S-4800 scanning electron microscope. The cell performance was tested using an electrochemical workstation (CHI 660E) and new wire (new) cell test system.
As can be seen from FIG. 1, the prepared CuSe sample had a pure hexagonal structure (JCPDS card No. 34-0171) in which no hetero peaks other than CuSe were detected. As can be seen from FIG. 2, the resulting products were of a sheet-like structure and varied in size. As can be seen from fig. 3, when the CuSe nano-sheet is used as an electrode material of a sodium ion battery for cyclic voltammetry, the cycle curves from the second circle to the fifth circle are basically coincident, which indicates that the nano-sheet has stable electrochemical performance. As can be seen from FIG. 4, the initial sodium storage specific capacity of the CuSe nano sheet can reach 425.2mAh/g, the initial coulomb efficiency is 96.9%, and the capacity is 335.1mAh/g after 120 charge and discharge cycles.
Drawings
FIG. 1 is an X-ray diffraction chart of a product obtained by a reaction for 1h at a temperature of 120℃in a hydrothermal synthesis reaction;
FIG. 2 is a scanning electron microscope image of the product obtained by the reaction for 1h at 120℃for the hydrothermal synthesis reaction.
Fig. 3 is a CV curve of a CuSe nanoplatelet material made according to an embodiment.
Fig. 4 is a cycle graph of a CuSe nanoplatelet material made according to an embodiment.
Detailed Description
1. 45.0mL of deionized water and 208.3mmol of sodium hydroxide are added into a 100mL reaction kettle, and after stirring and dissolving at room temperature, 3.2mmol of selenium powder is added;
2. after stirring at room temperature for 10min, 2.1mmol of cetyltrimethylammonium bromide and 2.0mmol of copper nitrate trihydrate were added;
3. after stirring for 10min at room temperature, the reaction kettle is placed in an oven, heated to 140 ℃ and kept for 1h, then cooled to room temperature, and subjected to centrifugal water washing and drying treatment, so that the pure flaky CuSe nano material can be obtained (see figures 1 and 2).
Claims (1)
1. The preparation method of the CuSe nanometer material for the sodium ion battery comprises the following steps:
a) Adding deionized water, sodium hydroxide and selenium powder into a 100mL reaction kettle in sequence;
b) Stirring for 10min, and adding cetyl trimethyl ammonium bromide and copper nitrate trihydrate;
c) Stirring for 10min, placing the reaction kettle in a baking oven, carrying out hydrothermal synthesis reaction at a specific temperature for a certain time, and carrying out centrifugal water washing and drying treatment to obtain the CuSe nano material;
the addition amounts of the selenium powder, the sodium hydroxide and the deionized water in the step a) are 3.2mmol, 208.3mmol and 45.0mL respectively;
the addition amounts of cetyl trimethyl ammonium bromide and copper nitrate trihydrate in the step b) are 2.1mmol and 2.0mmol respectively;
the temperature of the hydrothermal synthesis reaction in the step c) is 140 ℃, and the reaction time is 1-2h.
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