CN116062712A - Sodium battery current collector based on thorn-shaped copper nitride and preparation method and application thereof - Google Patents

Sodium battery current collector based on thorn-shaped copper nitride and preparation method and application thereof Download PDF

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CN116062712A
CN116062712A CN202310352181.3A CN202310352181A CN116062712A CN 116062712 A CN116062712 A CN 116062712A CN 202310352181 A CN202310352181 A CN 202310352181A CN 116062712 A CN116062712 A CN 116062712A
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current collector
copper
preparation
copper nitride
sodium
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李盼
郑子航
刘依凡
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Nanjing University of Posts and Telecommunications
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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
    • H01M4/64—Carriers or collectors
    • H01M4/66—Selection of materials
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/0615—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium
    • C01B21/0625—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with transition metals other than titanium, zirconium or hafnium with copper
    • 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
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/30—Particle morphology extending in three dimensions
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    • C01P2006/40—Electric properties
    • 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

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Abstract

The invention relates to a sodium battery current collector based on thorny copper nitride, a preparation method and application thereof. And nitriding the prepared copper oxide in a tube furnace. Preparation of sodium cell negative electrode current collector by taking copper nitride as material, ultrathin current collector prepared by thorn copper nitride, and 2mA/cm in high-capacity half-cell long-cycle test 2 Current density, capacity of 10mAh/cm 2 The coulomb efficiency of the pole piece is up to more than 98% after the pole piece circulates for 70 circles, and the thickness change of the pole piece is limited. The poleThe preparation method of the tablet is expandable and compatible with the industrialized process, and is a universal practical technology suitable for preparing the cathodes of other sodium batteries.

Description

Sodium battery current collector based on thorn-shaped copper nitride and preparation method and application thereof
Technical Field
The invention belongs to the technical field of energy storage batteries, and particularly relates to a sodium battery current collector based on thorn-shaped copper nitride, and a preparation method and application thereof.
Background
Due to the rarity and the uneven global distribution of lithium resources, researchers have found that the same family of elements, namely sodium, has similar physical and chemical properties to lithium, and sodium has large reserves and low cost. The electrode potential of sodium ions (Na/Na+) is 0.3V higher than that of lithium ions, the electrochemical performance is more stable, and the safety performance is higher.
However, sodium batteries also face various difficulties, on the one hand, the growth and volume expansion of sodium dendrites as the battery is cycled, resulting in reduced battery life; on the other hand, sodium ions have larger ion radius, and negative electrode materials for lithium batteries cannot remove sodium load, so that a negative electrode material suitable for sodium batteries needs to be searched.
Most three-dimensional current collectors have the defects of complicated preparation process and high quality of prepared pole pieces during design.
Disclosure of Invention
This section is intended to outline some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section as well as in the description summary and in the title of the application, to avoid obscuring the purpose of this section, the description summary and the title of the invention, which should not be used to limit the scope of the invention.
The present invention has been made in view of the above and/or problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a sodium battery current collector based on thorny copper nitride.
It is still another object of the present invention to overcome the deficiencies of the prior art and to provide a method for preparing a sodium battery current collector based on a copper nitride thorn.
In order to solve the technical problems, the invention provides a preparation method of a sodium battery current collector, which is characterized by comprising the following steps: the preparation method comprises the following steps of,
putting copper nano particles into a 1000 ml round-bottom flask, adding an ethanol solution with the volume fraction of 800 ml and 50%, and putting into ultrasonic equipment for ultrasonic treatment for 5 min to uniformly disperse nano copper.
The round bottom flask was placed in an oil bath at 72℃and a stabilizing oxygen gas was introduced.
After oil bath for 8 hours, suction filtration is carried out, and the filter cake is dried in a vacuum drying oven at 60 ℃ for 24 h.
Spreading the dried copper oxide in a porcelain boat, putting the porcelain boat into a tube furnace, introducing ammonia nitrogen mixed gas with the ammonia content of 30% and the flow of 200 sccm, filling a quartz tube, heating to 330 ℃, and keeping the temperature for 2.5 h. And after the reaction is finished, taking out a product after the ammonia nitrogen mixed gas atmosphere is reduced to room temperature, and obtaining the copper nitride.
As a preferred embodiment of the preparation process according to the invention, there is provided: and introducing oxygen to oxidize the copper nano particles, and growing copper oxide on the surface of the copper ball in situ.
As a preferred embodiment of the preparation process according to the invention, there is provided: the structure of the thorn-shaped copper oxide is kept complete after nitriding in a tube furnace.
As a preferred embodiment of the preparation process according to the invention, there is provided: the sodium battery current collector can be prepared into an ultrathin current collector, can be loaded with large capacity and has limited thickness variation of the pole piece.
It is still another object of the present invention to solve the deficiencies of the prior art and to provide a sodium battery current collector based on thorn copper nitride for use in an energy storage battery.
In order to solve the technical problems, the invention provides a preparation method of a sodium battery negative plate, which is characterized by comprising the following steps: the negative electrode material is prepared by mixing copper nitride, PVDF binder and carbon black according to the proportion of 8-4:2-1:2-1, and coating.
The invention has the beneficial effects that:
(1) The novel three-dimensional structure enhances the electric field intensity of the current collector and reduces the local current density. The nitrogen and oxygen elements in the solar cell actively guide the deposition of sodium, so that the deposition is more uniform, the growth of sodium dendrites is effectively inhibited, and the service life of the cell is prolonged.
(2) During the deposition process, the three-dimensional current collector stabilizes the formation of SEI, and simultaneously effectively inhibits sodium metal expansion through self dynamic change. Under the condition of large deposition quantity, the pole piece structure still remains complete and the thickness variation is limited.
(3) After the sodium is removed, the pole piece is restored to the original structure, and the reversibility is good. In addition, the pole piece is simple to manufacture, the cost is low, and the excellent electrochemical performance brings inspiration for designing a sodium negative electrode battery with better cycle stability.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art. Wherein:
FIG. 1 is an SEM image of the post-oxidation and nitridation morphology of Cu NPs; (a) copper oxide; (b) copper nitride;
fig. 2 is an XRD pattern of copper oxide and copper nitride.
Fig. 3 is a HRTEM image of copper nitride. (a) a TEM image; (b) an O element profile; (c) an N element profile; (d) Cu element profile;
FIG. 4 is a graph of Na@3DCu 3 PEIS and CV characterization graphs of N electrode half cells. (a) Na@3DCu 3 Impedance curve of the N electrode half cell; (b) Na@3DCu 3 CV curve of N electrode half cell;
FIG. 5 is a graph of Na@3DCu 3 N electrode half cell test pattern. (a) The current density was 2mA/cm -2 The capacity is 10mAh/cm -2 Coulomb efficiency contrast of (a); (b) the first-turn charge-discharge curve of fig. 5 (a);
FIG. 6 is an SEM image of the pole piece before and after deposition; (a) the thickness of the pole piece before deposition; (b) Deposit 3 mAh/cm -2 The thickness of the pole piece;
fig. 7 is an SEM image of the pole piece surface for different sodium deposition amounts. (a) 3D Cu 3 Deposition of N electrode sodium 1 mAh/cm -2 （b）3D Cu 3 N electrode sodium deposition 3 mAh/cm -2 (c) sodium copper foil deposition of 1 mAh/cm -2 (d) deposition of copper foil sodium 3 mAh/cm -2 。
Detailed Description
In order that the above-recited objects, features and advantages of the present invention will become more apparent, a more particular description of the invention will be rendered by reference to specific embodiments thereof which are illustrated in the appended drawings.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present invention is not limited to the specific embodiments disclosed below.
Further, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic can be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
(1) 300mg of Cu NPs are weighed, poured into a 1000 mL round bottom flask, 500 mL ultrapure water and 500 mL ethanol are weighed, sequentially poured into the round bottom flask, and ultrasonic treatment is performed for 5 min.
(2) The round bottom flask was placed in an oil bath at 72℃and a steady oxygen flow rate of 80 ml/min was introduced. Oil bath time 8 h.
(3) The solution from the round bottom flask was filtered off with suction, the filter cake was rinsed several times with ultra pure water and dried 24. 24 h in a vacuum oven at 60 ℃. The material was characterized using a scanning electron microscope and the results are shown in fig. 1a.
(4) And (5) placing the dried copper oxide into a tube furnace. And (3) discharging air in the tubular furnace by using an air pump, when the air pressure gauge P reaches a vacuum state (P= -1 MPa), introducing 30% ammonia nitrogen mixed gas, wherein the flow is a flushing state (maximum flow rate), when the air pressure gauge P is micro-positive pressure (P is more than or equal to 0 and less than or equal to 0.01 MPa), opening an air outlet, introducing air for 2 min, and then turning off the air pump, so that the flow of the ammonia nitrogen mixed gas is regulated to 150 sccm.
(5) After the quartz tube is filled with ammonia nitrogen mixed gas, a tube furnace program is set, the temperature is raised to 330 ℃ at 2 ℃/min, and the reaction is carried out at 2.5 h. Stopping heating after the reaction is finished, closing the ammonia nitrogen mixed gas, and taking out the product after the ammonia nitrogen mixed gas atmosphere is reduced to room temperature. The material was characterized using a scanning electron microscope and the results are shown in fig. 1b.
(6) Mixing copper nitride, PVDF binder and carbon black according to the proportion of 8:1:1, coating to prepare a pole piece, and placing in a glove box for standby.
The obtained copper oxide and copper nitride were subjected to XRD analysis, and the result was referred to fig. 2.
The HRTEM diagram of the resulting copper nitride is shown in fig. 3.
Preparation of sodium cell negative electrode current collector by taking copper nitride as material, ultrathin current collector prepared by thorn copper nitride, and 2mA/cm in high-capacity half-cell long-cycle test 2 Current density, capacity of 10mAh/cm 2 The coulomb efficiency of the pole piece is up to more than 98% after the pole piece circulates for 70 circles, and the thickness change of the pole piece is limited.
Example 2
(1) 500 mg of Cu NPs are weighed, poured into a 1000 mL round-bottomed flask, 500 mL ultrapure water and 500 mL ethanol are weighed, sequentially poured into the round-bottomed flask, and ultrasonic treatment is performed for 5 min.
(2) The round bottom flask was placed in an oil bath at 75℃and after 30 min of preheating, stable oxygen was introduced at a flow rate of 100 ml/min. Oil bath time 8 h.
(3) The solution from the round bottom flask was filtered off with suction, the filter cake was rinsed several times with ultra pure water and dried 24. 24 h in a vacuum oven at 60 ℃. The material was characterized using a scanning electron microscope and the results are shown in fig. 1a.
(4) And (5) placing the dried copper oxide into a tube furnace. And (3) discharging air in the tubular furnace by using an air pump, when the air pressure gauge P reaches a vacuum state (P= -1 MPa), introducing 30% ammonia nitrogen mixed gas, wherein the flow is a flushing state (maximum flow rate), when the air pressure gauge P is micro-positive pressure (P is more than or equal to 0 and less than or equal to 0.01 MPa), opening an air outlet, introducing air for 2 min, and then turning off the air pump, so that the flow of the ammonia nitrogen mixed gas is regulated to 150 sccm.
(5) After the quartz tube is filled with ammonia nitrogen mixed gas, a tube furnace program is set, the temperature is raised to 330 ℃ at 2 ℃/min, and the reaction is carried out at 2.5 h. Stopping heating after the reaction is finished, closing the ammonia nitrogen mixed gas, and taking out the product after the ammonia nitrogen mixed gas atmosphere is reduced to room temperature. The material was characterized using a scanning electron microscope and the results are shown in fig. 1b.
(6) Mixing copper nitride, PVDF binder and carbon black according to the proportion of 8:1:1, coating to prepare a pole piece, and placing in a glove box for standby.
Example 3
(1) 1g of Cu NPs was weighed, poured into a 1000 mL round bottom flask, 500 mL ultrapure water and 500 mL ethanol were measured, sequentially poured into the round bottom flask, and sonicated for 5 min.
(2) The round bottom flask was placed in an oil bath at 78℃and after 40 min of preheating, stable oxygen was introduced at a flow rate of 150 ml/min. Oil bath time 8 h.
(3) The solution from the round bottom flask was filtered off with suction, the filter cake was rinsed several times with ultra pure water and dried 24. 24 h in a vacuum oven at 60 ℃. The material was characterized using a scanning electron microscope and the results are shown in fig. 1a.
(4) And (5) placing the dried copper oxide into a tube furnace. And (3) discharging air in the tubular furnace by using an air pump, when the air pressure gauge P reaches a vacuum state (P= -1 MPa), introducing 30% ammonia nitrogen mixed gas, wherein the flow is a flushing state (maximum flow rate), when the air pressure gauge P is micro-positive pressure (P is more than or equal to 0 and less than or equal to 0.01 MPa), opening an air outlet, introducing air for 2 min, and then turning off the air pump, so that the flow of the ammonia nitrogen mixed gas is regulated to 150 sccm.
(5) After the quartz tube is filled with ammonia nitrogen mixed gas, a tube furnace program is set, the temperature is raised to 330 ℃ at 2 ℃/min, and the reaction is carried out at 2.5 h. Stopping heating after the reaction is finished, closing the ammonia nitrogen mixed gas, and taking out the product after the ammonia nitrogen mixed gas atmosphere is reduced to room temperature. The material was characterized using a scanning electron microscope and the results are shown in fig. 1b.
(6) Mixing copper nitride, PVDF binder and carbon black according to the proportion of 8:1:1, coating to prepare a pole piece, and placing in a glove box for standby.
Sodium battery electrode test was performed on the pole pieces prepared by coating in examples 1 to 3, wherein Na@3DCu 3 The PEIS and CV characterization diagrams of the N electrode half cell are shown in detail in FIG. 4, na@3DCu 3 The N-electrode half cell test chart is shown in fig. 5.
The state before and after the pole piece deposition was subjected to SEM analysis, wherein fig. 6 is an SEM image before and after the pole piece deposition, and fig. 7 is an SEM image of the pole piece surface with different sodium deposition amounts.
Along with the improvement of the quality of Cu NPs raw materials, the morphology of the thorn-shaped copper nitride is gradually changed, and the length of the thorn-shaped structure is shortened, because mutual competition is generated among Cu NPs, and part of raw materials cannot participate in the reaction, the original structure is still maintained, and the final performance of the product is influenced.
It should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered in the scope of the claims of the present invention.

Claims (10)

1. A preparation method of a sodium battery current collector based on thorn-shaped copper nitride is characterized by comprising the following steps: comprises the steps of,
adding copper nano particles into an ethanol solution, and uniformly dispersing by ultrasonic waves;
heating the mixed solution, and introducing oxygen for reaction;
carrying out suction filtration on the product, and drying a filter cake to obtain copper oxide;
and (3) introducing the dried copper oxide into ammonia nitrogen mixed gas for reaction to obtain copper nitride.
2. The method of manufacturing according to claim 1, wherein: the volume fraction of the ethanol solution is 30-70%.
3. The preparation method according to claim 1 or 2, characterized in that: the copper nanoparticle is added in an amount of 300mg to 1g.
4. A method of preparation as claimed in claim 3, wherein: and heating the mixed solution by adopting an oil bath, wherein the oil bath time is 6-10 hours.
5. The method of any one of claims 1, 2, and 4, wherein: the volume fraction of ammonia in the ammonia nitrogen mixed gas is 20-50%.
6. The method of manufacturing according to claim 5, wherein: the copper oxide is heated to 300-350 ℃ when being introduced into ammonia nitrogen mixed gas for reaction, and the reaction time is 1-4 hours.
7. A sodium battery current collector based on thorn copper nitride made by the method of claim 1.
8. Use of a sodium battery current collector based on spiny copper nitride according to claim 7 in an energy storage battery.
9. The use according to claim 8, wherein: the sodium battery current collector is used for preparing a sodium battery anode material.
10. The use according to claim 9, wherein: the cathode material is prepared by mixing copper nitride, PVDF binder and carbon black according to the proportion of 8-4:2-1:2-1, and forming paste, and coating.
CN202310352181.3A 2023-04-04 2023-04-04 Sodium battery current collector based on thorn-shaped copper nitride and preparation method and application thereof Pending CN116062712A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105826556A (en) * 2016-03-27 2016-08-03 华南理工大学 Ultrathin-layered NbS2, preparing method thereof and application of ultrathin-layered NbS2 to lithium/sodium-ion battery
CN111450867A (en) * 2020-05-09 2020-07-28 青岛科技大学 Cu for electrocatalytic carbon dioxide reduction3Preparation method of N nano catalyst
CN113725439A (en) * 2021-08-05 2021-11-30 武汉理工大学 Porous copper nitride nanowire array and preparation method and application thereof
CN114275745A (en) * 2021-12-06 2022-04-05 电子科技大学长三角研究院(湖州) Preparation method of copper nitride powder

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105826556A (en) * 2016-03-27 2016-08-03 华南理工大学 Ultrathin-layered NbS2, preparing method thereof and application of ultrathin-layered NbS2 to lithium/sodium-ion battery
CN111450867A (en) * 2020-05-09 2020-07-28 青岛科技大学 Cu for electrocatalytic carbon dioxide reduction3Preparation method of N nano catalyst
CN113725439A (en) * 2021-08-05 2021-11-30 武汉理工大学 Porous copper nitride nanowire array and preparation method and application thereof
CN114275745A (en) * 2021-12-06 2022-04-05 电子科技大学长三角研究院(湖州) Preparation method of copper nitride powder

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
徐凌, 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》, no. 2023 *

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