CN114156593B - Diaphragm functional material for improving performance of lithium metal battery, preparation and application - Google Patents
Diaphragm functional material for improving performance of lithium metal battery, preparation and application Download PDFInfo
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- CN114156593B CN114156593B CN202111439486.5A CN202111439486A CN114156593B CN 114156593 B CN114156593 B CN 114156593B CN 202111439486 A CN202111439486 A CN 202111439486A CN 114156593 B CN114156593 B CN 114156593B
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- 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
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- 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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- 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
- C01B32/182—Graphene
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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
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/431—Inorganic material
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- 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 discloses a diaphragm functional material for improving the electrochemical performance of a lithium metal battery, and preparation and application thereof, wherein the diaphragm functional material comprises the following steps: (1) dissolving sodium tungstate, potassium sulfate and sodium citrate in an aqueous solution containing graphene oxide, and (2) adjusting the pH of the solution; (3) pouring the mixture into a reaction kettle for hydrothermal reaction; (4) after the reaction is finished, cooling to room temperature, filtering, cleaning, and freeze-drying to obtain a precursor of the tungsten oxide and graphene oxide compound; (5) ammoniating the precursor in ammonia gas atmosphere, and cooling to room temperature to obtain the tungsten nitride embedded nitrogen-doped graphene nanoflowers; the invention firstly provides a method for synthesizing a tungsten precursor by a hydrothermal method assisted by a complexing surfactant, and then ammoniating to obtain the nitrogen-doped graphene nano flower powder embedded with tungsten nitride.
Description
Technical Field
The invention belongs to the technical field of nano material preparation and application in batteries, and particularly relates to a preparation method of tungsten nitride embedded nitrogen-doped graphene nanoflowers.
Background
In recent years, transition metal nitrides have been increasingly researched and applied to various industrial applications due to their unique characteristics of high melting point (>2000K), special hardness (>10GPa), good catalytic activity, chemical stability, radiation resistance, and the like, and have achieved certain results. Among the numerous known nitrides, boron, silicon, titanium and gallium nitride have gained extensive research and considerable attention, particularly in the electronic and semiconductor fields. However, although tungsten nitride has been successfully applied to stabilize sheet resistance and metal diffusion barriers, there has been little research on tungsten nitride and few reports on these nitrides. Therefore, most reports are about the deposition method of nitride thin film. Few reports have explored the synthesis of nanostructured forms of these nitrides chemically, which are more difficult to synthesize than the corresponding oxides, require strict anaerobic and anhydrous conditions and higher temperatures, which lead to grain growth and thus severely affect its nanoscale properties, especially of tungsten nitride. Therefore, it is significant to synthesize nano-sized tungsten nitride by a simple and mild method and to study its application in new fields, particularly in the field of energy storage. Meanwhile, the diaphragm is used as an important component of the battery and is required to have high mechanical strength, good thermal stability and high ion conductivity, so that the work of modifying the diaphragm of the lithium metal battery by using the transition metal nitride as a functional material to solve the problem of dendritic crystal growth of the lithium metal battery is of great significance.
In order to solve and overcome the problems, the invention provides a method for simply and efficiently preparing tungsten nitride embedded nitrogen-doped graphene (WNG) nanoflowers. Different complexing surfactants are utilized to construct a precursor easy to ammoniate, and the appearance, the embedded structure and the unique composition of the WNG nanoflower are constructed by adjusting the ammoniation temperature and time, so that the control of the performance is realized. The special structure and composition of WNG material endow the material with unique advantages: the nitrogen-doped graphene of the embedded layer serves as a supporting framework to provide structural stability of the whole material on one hand, and on the other hand, a channel is provided for rapid transmission of ions, meanwhile, embedded tungsten nitride provides a large number of active sites for uniform deposition of lithium ions due to strong polar functional groups of the tungsten nitride, so that local current density applied to a lithium cathode is reduced, and meanwhile, a stable solid electrolyte membrane is generated on the surface of the cathode, so that growth of lithium dendrites is inhibited, side reactions are relieved, the cycling stability of the battery is improved, and the utilization rate and the specific capacity of active substances are increased. The method disclosed by the invention has the advantages of green and environment-friendly experimental raw materials, low cost, simple experimental process and good repeatability, and provides a feasible preparation method for the application of the transition metal nitride composite material with the embedded structure in the lithium metal battery.
Disclosure of Invention
In view of the problems of the prior art, the invention provides a simple, effective, rapid and easy large-scale preparation method of the tungsten nitride embedded nitrogen-doped graphene nanoflower functional material, which can be applied to the field of energy storage.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a diaphragm functional material for improving the performance of a lithium metal battery is characterized by comprising the following steps:
step 1: taking 3-6 mmol of sodium tungstate, 6-14 mmol of potassium sulfate and 1-4 mmol of sodium citrate as raw materials, hydrochloric acid as a pH regulator and distilled water as a solvent;
step 2: dissolving the potassium sulfate, the sodium tungstate and the sodium citrate into 70mL of distilled water containing 60-100 mg of graphene oxide, stirring until the solid raw materials are completely dissolved, and adjusting the pH value to 1-2 by using hydrochloric acid to obtain a mixed solution;
and step 3: pouring the mixed solution obtained in the step 2 into a 100mL reaction kettle, and carrying out hydrothermal reaction at 160-200 ℃ for 18-36 hours; after the hydrothermal reaction is finished, naturally cooling to room temperature, filtering, cleaning, and freeze-drying to obtain a precursor of the tungsten oxide and graphene oxide compound;
and 4, step 4: weighing 0.5-1 g of the product obtained in the step (3), placing the product in a porcelain boat, heating to 600-700 ℃ at a heating rate of 2-5 ℃/min for 2-5 hours in a tubular furnace ammonia atmosphere, and cooling to room temperature to obtain the diaphragm functional material for improving the performance of the lithium metal battery.
Preferably, the heating rate of the tubular furnace ammoniation is 5 ℃/min to 550 ℃ from room temperature, and 2 ℃/min to 650 ℃ from 550 ℃.
Preferably, in the step 1, 5mmol of sodium tungstate, 10mmol of potassium sulfate and 2.5mmol of sodium citrate are used as raw materials.
Preferably, the pH is adjusted to 1.5 with hydrochloric acid.
Preferably, the concentration of hydrochloric acid for adjusting acidity is 3 to 6 mol/L.
The invention provides a diaphragm functional material for improving the performance of a lithium metal battery, which is a nitrogen-doped graphene nanoflower embedded with tungsten nitride.
The invention also provides application of the separator functional material for improving the performance of the lithium metal battery in the lithium metal battery, and the material is used for modifying the separator of the lithium metal battery.
Preferably, the material is used for improving the electrolyte wettability, the mechanical strength and the thermal stability of the lithium metal battery diaphragm, and improving the cycle stability and the rate capability of the lithium metal battery.
Preferably, the loading capacity of the diaphragm functional material is 0.138-0.310 mg/cm 2 。
Compared with the prior art, the invention has the following beneficial effects:
according to the method, cheap sodium citrate is used as a complexing surfactant, sodium tungstate is used as a tungsten source, hydrochloric acid is used as an acidity regulator, and a tungsten nitride-embedded nitrogen-doped graphene nanoflower is synthesized by combining an ammoniation process with a hydrothermal method for the first time;
the method provided by the invention has the characteristics of simple experimental process, low cost, strong repeatability and good controllability.
The synthesized material has good lithium affinity, high ionic conductivity, thermal stability and mechanical strength.
The lithium dendrite growth can puncture the diaphragm to cause battery short circuit, and the diaphragm modified by the synthesized functional material has high mechanical strength, so that the safety of the battery is improved from the mechanical perspective;
according to the embedded nanoflower structure prepared by the invention, the nitrogen-doped graphene of the embedded layer is used as a supporting framework, so that on one hand, the structural stability of the whole material is provided, on the other hand, a channel is provided for the rapid transfer of ions, and simultaneously, the embedded tungsten nitride provides a large number of active sites for the uniform deposition of lithium ions due to strong polar functional groups of the tungsten nitride, so that the local current density applied to a lithium cathode is reduced, and meanwhile, a stable solid electrolyte membrane is generated on the surface of the cathode, so that the growth of lithium dendrites is inhibited, side reactions are relieved, the cycling stability of a battery is improved, and the utilization rate and specific capacity of active substances are increased;
the nitrogen-doped graphene nanoflower functional material embedded with tungsten nitride, which is prepared by the invention, shows excellent electrochemical performance of the lithium metal battery due to the unique structure and composition, and provides a new idea for the design and application of the multifunctional diaphragm of the alkali metal battery.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention.
Fig. 2 is an X-ray diffraction pattern of tungsten nitride embedded nitrogen-doped graphene nanoflowers prepared in accordance with the present invention;
fig. 3 is a scanning electron microscope image of the tungsten nitride-embedded nitrogen-doped graphene nanoflower prepared according to the present invention;
FIG. 4 is an atomic force microscope Young's modulus distribution diagram of the nitrogen-doped graphene nanoflower modified membrane embedded with tungsten nitride prepared by the invention;
fig. 5 is an electrolyte contact angle diagram of the nitrogen-doped graphene nanoflower modified membrane embedded with tungsten nitride prepared by the present invention;
fig. 6 is a graph of the cycling stability performance of the nitrogen-doped graphene nanoflower modified membrane battery with tungsten nitride embedded according to the present invention.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Fig. 2 is an X-ray diffraction pattern of the tungsten nitride and the nitrogen-doped graphene nanoflower functional material embedded with the tungsten nitride prepared by the present invention, and it can be seen that the synthesized product is consistent with the standard peak of the tungsten nitride, which indicates that the tungsten nitride is successfully prepared.
Fig. 3 is a scanning electron microscope image of the nitrogen-doped graphene nanoflower embedded with tungsten nitride prepared by the present invention, and the nanoflower structure constructed by embedding tungsten nitride and nitrogen-doped graphene can be clearly seen from the image. Wherein (a) is a scanning electron micrograph at 1 μm; (b) is a scanning electron micrograph at 500 nm.
Fig. 4 is an atomic force microscope young's modulus distribution diagram of the nitrogen-doped graphene nanoflower modified diaphragm embedded with tungsten nitride prepared by the invention, and it can be seen that the bearing pressure ratio of the unmodified diaphragm is smaller, while the mechanical strength of the modified diaphragm is significantly improved, which is very beneficial to resisting the growth of lithium dendrites from a physical angle and improving the safety of the battery. Wherein, (a) is atomic force microscope young's modulus distribution diagram of unmodified diaphragm; (b) the Young's modulus distribution diagram of the atomic force microscope of the diaphragm modified by the functional material prepared by the invention.
Fig. 5 is a contact angle diagram of the electrolyte of the nitrogen-doped graphene nanoflower modified diaphragm embedded with tungsten nitride prepared by the invention, and it can be seen that the modified diaphragm has good wettability to the electrolyte compared with an unmodified diaphragm, which is very beneficial to the rapid transfer of lithium ions. Wherein (a) is an electrolyte contact angle diagram of an unmodified separator; (b) is an electrolyte contact angle diagram of the functional material modified diaphragm prepared by the invention.
Fig. 6 is a graph of the cycling stability of the nitrogen-doped graphene nanoflower modified diaphragm battery with embedded tungsten nitride prepared by the invention, and it can be seen that the battery packaged by the modified diaphragm has excellent cycling stability. Wherein (a) is a cycle stability chart at 1C for batteries packaged with unmodified separator and batteries packaged with functional material modified separator prepared by the present invention; (b) a cycle stability plot at 2C for unmodified separator packaged batteries and functional material modified separator packaged batteries prepared by the present invention; (c) cycling stability plots at 3C for unmodified separator packaged cells and functional material modified separator packaged cells prepared by the present invention.
Example 1
A preparation method of a diaphragm functional material for improving the performance of a lithium metal battery comprises the following steps:
step 1: taking 3mmol of sodium tungstate, 6mmol of potassium sulfate and 1mmol of sodium citrate as raw materials, hydrochloric acid as a pH regulator and distilled water as a solvent;
step 2: dissolving the potassium sulfate, the sodium tungstate and the sodium citrate into 70mL of distilled water containing 60mg of graphene oxide, stirring until the solid raw materials are completely dissolved, and then adjusting the pH to 1-2 by using hydrochloric acid to obtain a mixed solution, wherein the concentration of hydrochloric acid for adjusting the acidity is 3 mol/L;
and step 3: pouring the mixed solution obtained in the step 2 into a 100mL reaction kettle, and carrying out hydrothermal reaction at 160 ℃ for 18 hours; after the hydrothermal reaction is finished, naturally cooling to room temperature, filtering, cleaning, and freeze-drying to obtain a precursor of the tungsten oxide and graphene oxide compound;
and 4, step 4: weighing 0.5g of the product obtained in the step (3), placing the product in a porcelain boat, heating to 600 ℃ at a heating rate of 2-5 ℃/min for 2 hours in a tubular furnace ammonia atmosphere, and cooling to room temperature to obtain the diaphragm functional material for improving the performance of the lithium metal battery.
The functional material of the diaphragm for improving the performance of the lithium metal battery is a nitrogen-doped graphene nanoflower embedded with tungsten nitride.
The diaphragm functional material is applied to a lithium metal battery and used for modifying a lithium metal battery diaphragm, and the material is used for improving the electrolyte wettability, the mechanical strength and the thermal stability of the lithium metal battery diaphragm and improving the cycle stability and the rate capability of the lithium metal battery. The loading capacity of the diaphragm functional material is 0.138-0.310 mg/cm 2 。
Example 2
A preparation method of a diaphragm functional material for improving the performance of a lithium metal battery comprises the following steps:
step 1: taking 6mmol of sodium tungstate, 14mmol of potassium sulfate and 4mmol of sodium citrate as raw materials, hydrochloric acid as a pH regulator and distilled water as a solvent;
step 2: dissolving the potassium sulfate, the sodium tungstate and the sodium citrate into 70mL of distilled water containing 100mg of graphene oxide, stirring until the solid raw materials are completely dissolved, and then adjusting the pH to 1-2 by using hydrochloric acid to obtain a mixed solution, wherein the concentration of the hydrochloric acid for adjusting the acidity is 6 mol/L;
and step 3: pouring the mixed solution obtained in the step 2 into a 100mL reaction kettle, and carrying out hydrothermal reaction at 200 ℃ for 36 hours; after the hydrothermal reaction is finished, naturally cooling to room temperature, filtering, cleaning, and freeze-drying to obtain a precursor of the tungsten oxide and graphene oxide compound;
and 4, step 4: weighing 1g of the product obtained in the step 3, placing the product in a porcelain boat, heating the product to 700 ℃ in a tubular furnace at the heating rate of 5 ℃/min in the atmosphere of ammonia gas for 5 hours, cooling the product to room temperature, and obtaining the diaphragm functional material for improving the performance of the lithium metal battery.
The functional material of the diaphragm for improving the performance of the lithium metal battery is a nitrogen-doped graphene nanoflower embedded with tungsten nitride.
The functional material of the diaphragm of the embodiment is applied to a lithium metal battery and is used for modifying the diaphragm of the lithium metal battery, and the material is used for improving lithium metal electricityThe electrolyte wettability, mechanical strength and thermal stability of the cell diaphragm are improved, and the cycle stability and rate capability of the lithium metal battery are improved. The loading capacity of the diaphragm functional material is 0.138-0.310 mg/cm 2 。
Example 3
A preparation method of a diaphragm functional material for improving the performance of a lithium metal battery comprises the following steps:
step 1: taking 5mmol of sodium tungstate, 10mmol of potassium sulfate and 2.5mmol of sodium citrate as raw materials, hydrochloric acid as a pH regulator and distilled water as a solvent;
step 2: dissolving the potassium sulfate, the sodium tungstate and the sodium citrate into 70mL of distilled water containing 80mg of graphene oxide, stirring until the solid raw materials are completely dissolved, and adjusting the pH to 1.5 by using hydrochloric acid to obtain a mixed solution, wherein the concentration of hydrochloric acid for adjusting the acidity is 3-6 mol/L;
and step 3: pouring the mixed solution obtained in the step 2 into a 100mL reaction kettle, and carrying out hydrothermal reaction at 180 ℃ for 24 hours; after the hydrothermal reaction is finished, naturally cooling to room temperature, filtering, cleaning, and freeze-drying to obtain a precursor of the tungsten oxide and graphene oxide compound;
and 4, step 4: weighing 0.7g of the product obtained in the step 3, placing the product in a porcelain boat, heating the product from room temperature to 550 ℃ at the heating rate of 5 ℃/min in the atmosphere of tubular furnace ammonia gas, heating the product from 550 ℃ to 650 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 3 hours, and cooling the product to room temperature to obtain the diaphragm functional material for improving the performance of the lithium metal battery.
The functional material of the diaphragm for improving the performance of the lithium metal battery is a nitrogen-doped graphene nanoflower embedded with tungsten nitride.
The diaphragm functional material is applied to a lithium metal battery and used for modifying a lithium metal battery diaphragm, and the material is used for improving the electrolyte wettability, the mechanical strength and the thermal stability of the lithium metal battery diaphragm and improving the cycle stability and the rate capability of the lithium metal battery. The loading capacity of the diaphragm functional material is 0.138-0.310 mg/cm 2 。
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (9)
1. A preparation method of a diaphragm functional material for improving the performance of a lithium metal battery is characterized by comprising the following steps:
step 1: taking 3-6 mmol of sodium tungstate, 6-14 mmol of potassium sulfate and 1-4 mmol of sodium citrate as raw materials, hydrochloric acid as a pH regulator and distilled water as a solvent;
step 2: dissolving the potassium sulfate, the sodium tungstate and the sodium citrate into 70mL of distilled water containing 60-100 mg of graphene oxide, stirring until the solid raw materials are completely dissolved, and adjusting the pH value to 1-2 by using hydrochloric acid to obtain a mixed solution;
and step 3: pouring the mixed solution obtained in the step 2 into a 100mL reaction kettle, carrying out hydrothermal reaction at 160-200 ℃ for 18-36 hours, naturally cooling to room temperature after the hydrothermal reaction is finished, filtering, cleaning, and freeze-drying to obtain a precursor of the tungsten oxide and graphene oxide compound;
and 4, step 4: weighing 0.5-1 g of the product obtained in the step (3), placing the product in a porcelain boat, heating to 600-700 ℃ at a heating rate of 2-5 ℃/min for 2-5 hours in a tubular furnace ammonia atmosphere, and cooling to room temperature to obtain the diaphragm functional material for improving the performance of the lithium metal battery.
2. The method for preparing a separator functional material for improving performance of a lithium metal battery according to claim 1, wherein: the heating rate of the tubular furnace ammoniation is 5 ℃/min to 550 ℃ from room temperature, and 2 ℃/min to 650 ℃ from 550 ℃.
3. The method for preparing a separator functional material for improving performance of a lithium metal battery according to claim 1, wherein: in the step 1, 5mmol of sodium tungstate, 10mmol of potassium sulfate and 2.5mmol of sodium citrate are used as raw materials.
4. The method for preparing a separator functional material for improving performance of a lithium metal battery according to claim 1, wherein: the pH was adjusted to 1.5 with hydrochloric acid.
5. The method for preparing a separator functional material for improving performance of a lithium metal battery according to claim 1, wherein: the concentration of hydrochloric acid for adjusting acidity is 3-6 mol/L.
6. The separator functional material for improving the performance of a lithium metal battery obtained by the method of any one of claims 1 to 5, characterized in that: the material is a nitrogen-doped graphene nanoflower embedded with tungsten nitride.
7. Use of the separator functional material for improving performance of a lithium metal battery according to claim 6 in a lithium metal battery, wherein: the material is used for modifying a separator of a lithium metal battery.
8. Use of the separator functional material for improving the performance of a lithium metal battery according to claim 7 in a lithium metal battery, characterized in that: the material is used for improving the electrolyte wettability, the mechanical strength and the thermal stability of the lithium metal battery diaphragm, and improving the cycle stability and the rate capability of the lithium metal battery.
9. Use of the separator functional material for improving the performance of a lithium metal battery according to claim 7 in a lithium metal battery, characterized in that: the loading capacity of the diaphragm functional material is 0.138-0.310 mg/cm 2 。
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