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CN113394381A - Preparation method of layered double hydroxide composite material for positive electrode of lithium-sulfur battery - Google Patents

Preparation method of layered double hydroxide composite material for positive electrode of lithium-sulfur battery Download PDF

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CN113394381A
CN113394381A CN202110645568.9A CN202110645568A CN113394381A CN 113394381 A CN113394381 A CN 113394381A CN 202110645568 A CN202110645568 A CN 202110645568A CN 113394381 A CN113394381 A CN 113394381A
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methanol
feconi
composite material
lithium
solution
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CN113394381B (en
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王新
胡晨晨
宋延丽
韦小玲
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Zhaoqing South China Normal University Optoelectronics Industry Research Institute
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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
    • H01M4/364—Composites as mixtures
    • 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
    • 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
    • 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
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • H01M2004/028—Positive 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
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a preparation method of a layered double hydroxide composite material for a lithium-sulfur battery anode. The preparation method of the layered double hydroxide composite material for the positive electrode of the lithium-sulfur battery comprises the following steps: (1) synthesizing AC-FeCoNi; (2) synthesizing Cu SAs/AC-FeCoNi. Copper atoms are introduced into AC-FeCoNi through an in-situ cation exchange reaction to prepare the Cu SAs/AC-FeCoNi composite material, and the preparation method is simple, effective and easy to operate; the prepared composite material has high conductivity, high specific surface area and stable three-dimensional structure.

Description

Preparation method of layered double hydroxide composite material for positive electrode of lithium-sulfur battery
Technical Field
The invention belongs to the technical field of lithium-sulfur batteries, and particularly relates to a preparation method of a layered double hydroxide composite material for a lithium-sulfur battery anode.
Background
In recent years, with the rapid development of our country's industry, the briskly developed Lithium Sulfur Battery (LSB) has been enriched with lithium (3860mAh &)-1) And Sulfur (1672 mAh. et. g-1) Becomes one of the most promising next-generation energy storage systems due to its remarkable theoretical specific capacity. Earth's rich sulfur has the advantages of low cost and environmental friendliness, however, practical application of LSB is still subject to low sulfur utilization ((S))<80%) and limited lifetime: (<500 cycles), mainly due to S/Li2Poor conductivity of S and the effect of shuttle effects. In addition, the slow conversion kinetics of polysulfides (LiPSs) and the accompanying large volume fluctuations lead to poor coulombic efficiency and cycle stability.
In order to solve the above problems, various carbon materials (carbon nanotubes, graphene, mesoporous carbon, etc.) are considered as good matrix materials for sulfur cathodes due to good electrical conductivity and various structural morphologies. However, they do not effectively inhibit the shuttling effect because they only weakly physically adsorb dissolved polysulfides. Considering that polysulfide is essentially a polar substance, metal compounds with abundant polar active centers are also widely studied, and it is very important to rationally design the multifunctional LSB cathode as a sulfur host and a LiPSs mediator. Polar transition metals (e.g. Co), metal nitrides (e.g. TiN and Co)4N), metal sulfides (e.g. Co)9S8And SnS2) And layered double hydroxides (e.g., NiCo-LDH and NiFe-LDH) have been shown to be effective multifunctional LSB cathodes, capturing LiPSs and promoting LiPSs conversion kinetics. Simple binding of polar sites still shows limited active sites and poor conductivity, resulting in a rapid decrease in capacity over an extended lifetime. To address this problem, tailoring and constructing a well-arranged multicomponent heterostructure can expose more active sites and improve conductivity, thereby improving sulfur utilization and mitigating capacity fade in long charge-discharge cycles. At present, the prior art is dedicated to effectively improve the catalytic activity of the carbon material by dispersing metal monoatomic atoms, but researches on compounding polar metal compounds and metal monoatomic atoms are rare.
Disclosure of Invention
The invention aims to provide a preparation method of a layered double hydroxide composite material for a lithium-sulfur battery anode, aiming at the existing defects, copper atoms are introduced into AC-FeCoNi through an in-situ cation exchange reaction to prepare a Cu SAs/AC-FeCoNi composite material, and the preparation method is simple, effective and easy to operate; the prepared composite material has high conductivity, high specific surface area and stable three-dimensional structure.
The technical scheme of the invention is as follows: a preparation method of a layered double hydroxide composite material for a positive electrode of a lithium-sulfur battery comprises the following steps:
(1) synthesis of AC-FeCoNi: firstly, NiCl is added2·6H2O and FeCl2Dissolving in methanol to obtain methanol solution A for later use; ultrasonically dispersing ZIF-67 in methanol to obtain a methanol solution B; then pouring the methanol solution A into the methanol solution B, and fully stirring to obtain a mixed solution; finally, transferring the mixed solution into an autoclave, heating for 1h at 120 ℃, centrifuging, collecting a product, washing by using methanol to remove residual ions, and freeze-drying for 12 h;
(2) synthesis of Cu SAs/AC-FeCoNi: ultrasonically dispersing the AC-FeCoNi obtained in the step (1) in a methanol/ammonium hydroxide mixture to obtain an AC-FeCoNi solution; adding CuCl2·H2Dissolving O in methanol to obtain CuCl2A methanol solution; under the condition of continuous stirring at room temperature, CuCl is added2Dropwise adding a methanol solution into an AC-FeCoNi solution, and carrying out ultrasonic treatment at room temperature for 30-60 minutes to obtain a mixture; after further heating the mixture at 60 ℃ for 10 hours, the product was collected by centrifugation, washed with methanol to remove residual ions, and freeze-dried for 12 hours to obtain Cu SAs/AC-FeCoNi.
The prepared Cu SAs/AC-FeCoNi is of a hollow nano-frame structure, and a single Cu atom is uniformly dispersed above the AC-FeCoNi; the amorphous outer layer in the Cu SAs/AC-FeCoNi consists of a defect site and an unsaturated coordination site and is used as an anchoring site for stabilizing a single Cu atom; the interior of the crystal has a highly symmetrical rigid structure.
NiCl in the step (1)2·6H2190.1-383 mg of O and FeCl2Is 25.4-50.9 mg of the two are dissolved in 20-40 mL of methanol; 50-100 mg of ZIF-67, and dissolving the ZIF-67 in 10-20 mL of methanol.
In the step (2), the amount of AC-FeCoNi is 40-80 mg; the methanol/ammonium hydroxide mixture is 20-40 mL, wherein the mass ratio of methanol: ammonium hydroxide is 3: 1; CuCl2·H2O is 1.0-2.0 mg and CuCl2·H2Dissolving O in 5-10 mL of methanol.
And (2) stirring the methanol solution A and the methanol solution B for 30 minutes in the step (1).
The invention has the beneficial effects that: the invention introduces Cu atoms into AC-FeCoNi through an in-situ cation exchange reaction to prepare a single Cu atom composite material loaded by mixed amorphous/crystalline FeCoNi LDH. The copper monatomic doped mixed amorphous/crystalline FeCoNi layered double hydroxide composite material prepared by the preparation method has the following characteristics:
(1) the Cu SAs/AC-FeCoNi has a unique cubic structure, and the layered double hydroxide of the Cu SAs/AC-FeCoNi can improve the specific surface area of the composite material and is beneficial to improving the loading amount of active substances.
(2) Cu SAs/AC-FeCoNi has a hybrid structure of amorphous and crystalline LDHs, possesses a stable balance than amorphous materials when exposed to highly corrosive and oxidative environments, and optimizes stability and activity. After the self-template cation exchange method, Layered Double Hydroxides (LDH) are obtained, because the layered double hydroxides have abundant hydrophilic hydroxyl groups and have strong chemical affinity to LiPSs, and through enough 'thiophilic' sites, the ultrahigh specific surface area increases more active sites, which is beneficial to improving the adsorption effect of the composite material on polysulfide in the electrochemical reaction process.
(3) The Cu SAs/AC-FeCoNi has high stability, and an amorphous outer layer in the Cu SAs/AC-FeCoNi consists of rich defect sites and unsaturated coordination sites and can be used as an anchoring site for fixing a single Cu atom. The crystal has a highly symmetrical rigid structure inside, thereby enhancing the stability of the support and thus helping to alleviate the volume expansion effect of the active material during the reaction.
(4) Cu SAs/AC-FeCoNi has high catalytic performance, and copper atoms are embedded into the AC-FeCoNi through strong metal-carrier interaction, so that local electronic configuration and internal electronic rearrangement are triggered. The doping of the metal copper atom obviously influences the coordination environment and symmetry of the cobalt atom center, thereby greatly improving the intrinsic activity of the cobalt active center. Therefore, the rate of conversion of polysulfides can be effectively promoted during the electrochemical reaction of the lithium sulfur battery, while the chemisorption with polysulfides is enhanced. These excellent properties lead to enhanced active material utilization and cycle performance of lithium sulfur batteries.
The invention adopts a simple solvent method and an in-situ cation exchange method to prepare the copper monatomic doped mixed amorphous/crystalline FeCoNi layered double hydroxide composite material, and the method has the characteristics of low cost and simple preparation process.
Drawings
FIG. 1 is an electrochemical specific capacity curve of the Cu SAs/AC-FeCoNi composite material as a positive electrode material for a lithium-sulfur battery in example 1.
FIG. 2 is the electrochemical specific capacity curve of the Cu SAs/AC-FeCoNi composite material as a positive electrode material for a lithium-sulfur battery in example 2.
Detailed Description
The present invention will be described in detail below with reference to examples.
Example 1
The preparation method of the layered double hydroxide composite material for the positive electrode of the lithium-sulfur battery comprises the following steps:
(1) synthesis of AC-FeCoNi: 190.1mgNiCl is first added2·6H2O and 25.4mgFeCl2Dissolving in 20mL of methanol to obtain a methanol solution A for later use; ultrasonically dispersing 50mgZIF-67 in 10mL of methanol to obtain a methanol solution B; then pouring the methanol solution A into the methanol solution B, and stirring for 30 minutes to obtain a mixed solution; finally, transferring the mixed solution into an autoclave, heating for 1h at 120 ℃, centrifuging, collecting a product, washing by using methanol to remove residual ions, and freeze-drying for 12 h;
(2) synthesis of Cu SAs/AC-FeCoNi: subjecting the product of step (1)Obtaining 40mgAC-FeCoNi (amorphous/crystalline FeCoNi LDH hollow nano-box) and ultrasonically dispersing in 20mL methanol/ammonium hydroxide mixture to obtain AC-FeCoNi solution, wherein the mass ratio of methanol: ammonium hydroxide is 3: 1; adding 1.0mgCuCl2﹒H2Dissolving O in 5mL of methanol to obtain CuCl2A methanol solution; under the condition of continuous stirring at room temperature, CuCl is added2Dropwise adding a methanol solution into an AC-FeCoNi solution, and carrying out ultrasonic treatment at room temperature for 30 minutes to obtain a mixture; after further heating the mixture at 60 ℃ for 10 hours, the product was collected by centrifugation, washed with methanol to remove residual ions, and freeze-dried for 12 hours to obtain Cu SAs/AC-FeCoNi.
Example 2
In the step (2) for synthesizing the Cu SAs/AC-FeCoNi, CuCl is added under the condition of continuous stirring at room temperature2The methanol solution was added dropwise to the AC-FeCoNi solution, and sonicated at room temperature for 50 minutes to give a mixture.
The rest is the same as in example 1.
Example 3
The preparation method of the layered double hydroxide composite material for the positive electrode of the lithium-sulfur battery comprises the following steps:
(1) synthesis of AC-FeCoNi: first 383mgNiCl2·6H2O and 50.9mgFeCl2Dissolving in 40mL of methanol to obtain a methanol solution A for later use; ultrasonically dispersing 100mgZIF-67 in 20mL of methanol to obtain a methanol solution B; then pouring the methanol solution A into the methanol solution B, and stirring for 30 minutes to obtain a mixed solution; finally, transferring the mixed solution into an autoclave, heating for 1h at 120 ℃, centrifuging, collecting a product, washing by using methanol to remove residual ions, and freeze-drying for 12 h;
(2) synthesis of Cu SAs/AC-FeCoNi: ultrasonically dispersing 80mg of AC-FeCoNi obtained in the step (1) in 40mL of methanol/ammonium hydroxide mixture to obtain an AC-FeCoNi solution, wherein the mass ratio of methanol: ammonium hydroxide is 3: 1; 2.0mg of CuCl2﹒H2Dissolving O in 10mL of methanol to obtain CuCl2A methanol solution; under the condition of continuous stirring at room temperature, CuCl is added2Adding methanol solution into AC-FeCoNi solution drop by drop, and performing ultrasonic treatment at room temperature for 60 minutes to obtainTo a mixture; after further heating the mixture at 60 ℃ for 10 hours, the product was collected by centrifugation, washed with methanol to remove residual ions, and freeze-dried for 12 hours to obtain Cu SAs/AC-FeCoNi.

Claims (5)

1. A preparation method of a layered double hydroxide composite material for a positive electrode of a lithium-sulfur battery is characterized by comprising the following steps of:
(1) synthesis of AC-FeCoNi: firstly, NiCl is added2·6H2O and FeCl2Dissolving in methanol to obtain methanol solution A for later use; ultrasonically dispersing ZIF-67 in methanol to obtain a methanol solution B; then pouring the methanol solution A into the methanol solution B, and fully stirring to obtain a mixed solution; finally, transferring the mixed solution into an autoclave, heating for 1h at 120 ℃, centrifuging, collecting a product, washing by using methanol to remove residual ions, and freeze-drying for 12 h;
(2) synthesis of Cu SAs/AC-FeCoNi: ultrasonically dispersing the AC-FeCoNi obtained in the step (1) in a methanol/ammonium hydroxide mixture to obtain an AC-FeCoNi solution; adding CuCl2·H2Dissolving O in methanol to obtain CuCl2A methanol solution; under the condition of continuous stirring at room temperature, CuCl is added2Dropwise adding a methanol solution into an AC-FeCoNi solution, and carrying out ultrasonic treatment at room temperature for 30-60 minutes to obtain a mixture; after further heating the mixture at 60 ℃ for 10 hours, the product was collected by centrifugation, washed with methanol to remove residual ions, and freeze-dried for 12 hours to obtain Cu SAs/AC-FeCoNi.
2. The method for preparing a layered double hydroxide composite material for a lithium-sulfur battery positive electrode according to claim 1, wherein the prepared Cu SAs/AC-FeCoNi has a hollow nano-frame structure, and a single Cu atom is uniformly dispersed over the AC-FeCoNi; the amorphous outer layer in the Cu SAs/AC-FeCoNi consists of a defect site and an unsaturated coordination site and is used as an anchoring site for stabilizing a single Cu atom; the interior of the crystal has a highly symmetrical rigid structure.
3. The lithium sulfur battery according to claim 1The preparation method of the layered double hydroxide composite material of the anode is characterized in that NiCl is adopted in the step (1)2·6H2190.1-383 mg of O and FeCl225.4-50.9 mg, and the two are dissolved in 20-40 mL of methanol; 50-100 mg of ZIF-67, and dissolving the ZIF-67 in 10-20 mL of methanol.
4. The method for preparing a layered double hydroxide composite material for a positive electrode of a lithium-sulfur battery according to claim 1, wherein the amount of AC-FeCoNi in the step (2) is 40 to 80 mg; the methanol/ammonium hydroxide mixture is 20-40 mL, wherein the mass ratio of methanol: ammonium hydroxide is 3: 1; CuCl2·H2O is 1.0-2.0 mg and CuCl2·H2Dissolving O in 5-10 mL of methanol.
5. The method for preparing a layered double hydroxide composite material for a positive electrode of a lithium sulfur battery according to claim 1, wherein the methanol solution a and the methanol solution B are stirred for 30 minutes in the step (1).
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CN115074750A (en) * 2022-07-29 2022-09-20 陕西科技大学 Nickel monoatomic/AlN co-inlaid carbon nanotube electrocatalyst and preparation method thereof

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