CN113394381B - 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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CN113394381B
CN113394381B CN202110645568.9A CN202110645568A CN113394381B CN 113394381 B CN113394381 B CN 113394381B CN 202110645568 A CN202110645568 A CN 202110645568A CN 113394381 B CN113394381 B CN 113394381B
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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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    • 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
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    • 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
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    • 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
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    • 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
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    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
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    • Y02E60/10—Energy storage using batteries

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; and (2) synthesizing Cu SAs/AC-FeCoNi. Copper atoms are introduced into the 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
Recently, with the rapid development of our country's industry, the brisk Lithium Sulfur Battery (LSB) has evolved due to its lithium (3860 mAh & -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-rich sulfur has the advantages of low cost and environmental friendliness, however, practical application of LSB is still subject to low sulfur utilization: (<80%) and limited lifetime: (<500 cycles), mainly due to S/Li 2 Poor conductivity of S and the effect of shuttle effects. In addition, the kinetics of conversion of polysulfides (LiPSs) are retardedSlow and 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) 4 N), metal sulfides (e.g. Co) 9 S 8 And SnS 2 ) 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 added 2 ·6H 2 O and FeCl 2 Dissolving 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 CuCl 2 ·H 2 Dissolving O in methanol to obtain CuCl 2 A methanol solution; under the condition of continuous stirring at room temperature, cuCl is added 2 Dropwise adding a methanol solution into the 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 single Cu atoms are 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 ·6H 2 O is 190.1 to 383mg 2 25.4-50.9 mg, and the two are dissolved in 20-40 mL of methanol; ZIF-67 was 50-100mg, and ZIF-67 was dissolved in 10-20 mL of methanol.
The amount of the AC-FeCoNi in the step (2) is 40-80 mg; the methanol/ammonium hydroxide mixture is 20-40 mL, wherein the mass ratio of methanol: ammonium hydroxide is 3; cuCl 2 ·H 2 O is 1.0-2.0mg, cuCl 2 ·H 2 O is dissolved 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: according to the invention, cu atoms are introduced 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) The Cu SAs/AC-FeCoNi has a hybrid structure of amorphous and crystalline LDHs, possesses a stable balance when exposed to highly corrosive and oxidative environments than amorphous materials 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 abundant 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 support and thus helping to alleviate the effect of volume expansion 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 by 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 added 2 ·6H 2 O and 25.4mgFeCl 2 Dissolving 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) Synthesizing Cu SAs/AC-FeCoNi: ultrasonically dispersing 40mg of AC-FeCoNi (amorphous/crystalline FeCoNi LDH hollow nano box) obtained in the step (1) in 20mL of methanol/ammonium hydroxide mixture to obtain an AC-FeCoNi solution, wherein the mass ratio of methanol: ammonium hydroxide is 3; adding 1.0mgCuCl 2 ﹒H 2 Dissolving O in 5mL of methanol to obtain CuCl 2 A methanol solution; under the condition of continuous stirring at room temperature, adding CuCl 2 Dropwise adding a methanol solution into the AC-FeCoNi solution, and carrying out ultrasonic treatment at room temperature for 30 minutes to obtain a mixture; after the mixture was further heated at 60 ℃ for 10 hours, the product was collected by centrifugation and washed with methanol to removeResidual ions are frozen and 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 temperature 2 The 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) Synthesizing AC-FeCoNi: first 383mgNiCl 2 ·6H 2 O and 50.9mgFeCl 2 Dissolving 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) Synthesizing 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; 2.0mg of CuCl 2 ﹒H 2 Dissolving O in 10mL of methanol to obtain CuCl 2 A methanol solution; under the condition of continuous stirring at room temperature, adding CuCl 2 Dropwise adding a methanol solution into the AC-FeCoNi solution, and performing ultrasonic treatment at room temperature for 60 minutes to obtain a mixture; after the mixture was further heated 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 (4)

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 added 2 ·6H 2 O and FeCl 2 Dissolved in methanolObtaining 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 CuCl 2 ·H 2 Dissolving O in methanol to obtain CuCl 2 A methanol solution; under the condition of continuous stirring at room temperature, adding CuCl 2 Dropwise adding a methanol solution into the AC-FeCoNi solution, and carrying out ultrasonic treatment at room temperature for 30-60 minutes to obtain a mixture; further heating the mixture at 60 ℃ for 10 hours, centrifuging to collect a product, washing with methanol to remove residual ions, and freeze-drying for 12 hours to obtain Cu SAs/AC-FeCoNi;
the prepared Cu SAs/AC-FeCoNi is of a hollow nano-frame structure, and single Cu atoms are 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.
2. The method for preparing a layered double hydroxide composite material for a positive electrode of a lithium sulfur battery according to claim 1, wherein NiCl is added in the step (1) 2 ·6H 2 O is 190.1 to 383mg 2 25.4-50.9 mg, and the two are dissolved in 20-40 mL of methanol; ZIF-67 is 50-100mg, and ZIF-67 is dissolved in 10-20 mL of methanol.
3. 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 AC-FeCoNi in the step (2) is 40 to 80mg; the methanol/ammonium hydroxide mixture is 20-40 mL, wherein the mass ratio of methanol: ammonium hydroxide is 3; cuCl 2 ·H 2 O is 1.0-2.0 mg, cuCl 2 ·H 2 O is dissolved in 5-10 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 methanol solution a and the methanol solution B are stirred for 30 minutes in the step (1).
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