CN113036121B - Carbon-coated transition metal sulfide nanoflower structure, preparation method and application thereof - Google Patents
Carbon-coated transition metal sulfide nanoflower structure, preparation method and application thereof Download PDFInfo
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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
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Abstract
The invention provides a carbon-coated transition metal sulfide nanoflower structure, a preparation method and application thereof, and belongs to the technical field of lithium ion batteries. The preparation process comprises the steps of firstly converting a spherical glycerin metal complex into a flower-shaped structure by a solvothermal method, then carrying out polymerization coating on the outer layer by taking dopamine hydrochloride as a carbon source, and finally carrying out high-temperature vulcanization to form a transition metal sulfide and simultaneously carbonizing polydopamine to obtain the carbon-coated transition metal sulfide nanoflower structure. The preparation method is simple, the conditions are mild, and the morphology of the product is easy to control. The prepared carbon-coated transition metal sulfide nanoflower structure can effectively relieve stress change in the charging and discharging process, reduces structural damage and has excellent electrochemical performance.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and relates to a carbon-coated transition metal sulfide nanoflower structure and a preparation method thereof.
Background
The lithium ion battery has the advantages of high voltage, large energy density, small pollution and the like, but the performance of the lithium ion battery is difficult to meet the application in the field of energy storage. The development and application of the negative electrode material are one of the ways to improve the performance of the lithium ion battery. Compared with the commercialized graphite cathode material, the transition metal sulfide has abundant oxidation-reduction reaction sites, so that the specific capacity of the transition metal sulfide is several times that of the graphite cathode material. However, the large volume expansion and the severe pulverization phenomenon of the lithium ion battery also have large influence on the electrochemical performance of the lithium ion battery.
The construction of suitable nanostructures and their complexation with carbon materials has been shown to improve the electrochemical performance of transition metal sulphides. The most widely used methods for preparing transition metal sulfides with various shapes are a template method and a chemical vapor deposition method, and the methods are complex and tedious to operate and are not easy to control the shapes. Yang, et al [ Nanoscale adv.2020,2,512 ] use SiO2Ball as template, SiO2Ball preparation-phenolic aldehyde coating-solvothermal-calcining-etching-sulfurizing to prepare NiS2A helmet-like carbon structure with nano-particles embedded; liu, et al [ Energy Environ Sci.2017.10.1576 ] utilizes Fe2O3As a template, by Fe2O3Preparation of nanocubes-polydopamine coating-calcination-partial etching-vulcanization to prepare FeS2@ C yolk-shell nanocube structure; liang, et al [ adv. energy mater.2017.7.1701309 ] self-supporting NiS was prepared using chemical vapor deposition2/FeS2A porous sheet-like structure. Therefore, it is important to obtain a material with excellent properties by improving stability through a simple and mild method, which is also the focus of current research.
Disclosure of Invention
Aiming at the problem that the preparation process of the transition metal sulfide and carbon composite material is complex, the invention provides a simple and mild method for preparing a carbon-coated transition metal sulfide nanoflower structure; converting the spherical glycerol metal complex into a flower-like structure by a solvothermal method; coating a polydopamine layer outside, and carrying out high-temperature vulcanization to obtain a carbon-coated transition metal sulfide; the nano flower structure can provide effective buffer space for the volume expansion of the transition metal sulfide generated in the charge and discharge process of the battery, so that the battery obtains excellent electrochemical performance.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a carbon-coated transition metal sulfide nanometer flower structure takes a flower-shaped structure obtained by a spherical glycerin metal complex through a solvothermal reaction as a template; polymerizing dopamine hydrochloride serving as a carbon source on the surface of the flower-shaped structure to form a shell; and (3) taking sulfur powder as a sulfur source, and carbonizing the polydopamine while vulcanizing at high temperature to obtain the transition metal sulfide to obtain the carbon-coated transition metal sulfide nanoflower structure.
A preparation method of a carbon-coated transition metal sulfide nanoflower structure comprises the following steps:
in the first step, a metal salt is added to a mixed solvent of glycerin and isopropanol at room temperature, wherein 0.2-1g of the metal salt is added to every 80ml of the mixed solvent. Fully stirring until the mixture is dissolved, transferring the mixture into a high-temperature high-pressure reaction kettle, reacting for 4 to 12 hours at the temperature of between 160 and 200 ℃, and naturally cooling the mixture to room temperature, and then carrying out alcohol washing, centrifugation and drying to obtain a glycerol metal complex sample.
And a second step of adding the glycerol metal complex to a mixed solvent of water and ethanol, wherein 0.08-0.5g of the glycerol metal complex is added to each 150mL of the mixed solvent. And (3) carrying out ultrasonic treatment for a period of time, transferring the mixture into a high-temperature high-pressure reaction kettle, reacting for 6-24h at the temperature of 100-180 ℃, and after naturally cooling to room temperature, carrying out water washing, alcohol washing, centrifugation and drying to obtain a solvothermal sample.
And thirdly, adding the solvent thermal sample, dopamine hydrochloride and tris (hydroxymethyl) aminomethane into a proper amount of water, stirring and reacting for 6-24h at room temperature, and performing water washing, alcohol washing, centrifugation and drying to obtain a polydopamine coated sample. Wherein, every 80-160mL of water is correspondingly added with: 0.1-0.3g of solvothermal sample, 0.05-0.25g of dopamine hydrochloride and 0.06-0.15g of tris (hydroxymethyl) aminomethane.
And fourthly, mixing the polydopamine coated sample with sulfur powder in a certain proportion, transferring the mixture into a ceramic square boat, then carrying out vulcanization treatment in a tube furnace under the protection of argon gas, carrying out vulcanization treatment at the temperature of 250-600 ℃ for 4-12h, and taking out the sample after the vulcanization treatment is finished under the protection of inert gas until the sample is naturally cooled, thus obtaining the carbon-coated transition metal sulfide material.
Further, in the first step, the metal salt is one of cobalt nitrate, nickel nitrate, cobalt acetate, nickel acetate, cobalt chloride, nickel chloride and a combination thereof.
Further, the volume ratio of glycerol to isopropanol in the mixed solvent in the first step is 1: 3-1: 7.
further, the volume ratio of ethanol to water in the mixed solvent in the second step is 1: 0.5-1: 4.
furthermore, the ultrasonic time in the second step is 10-30 min.
Further, the mass ratio of the polydopamine-coated sample to the sulfur powder in the fourth step is 1: 3-1: 20.
an application of a carbon-coated transition metal sulfide nanoflower structure can be used as a negative active material of a lithium ion battery. The preparation method of the negative plate comprises the following steps of respectively adopting acetylene black as a conductive agent, polyvinylidene fluoride (PVDF) as a binder and a small amount of N-methylpyrrolidone (NMP) as a solvent, wherein the mass ratio of the active material to the acetylene black to the PVDF is as follows: 8: 1: 1, after magnetic stirring for 12 hours, uniformly coating the copper foil, drying the copper foil in a vacuum oven at 120 ℃ for 12 hours, and punching the sample into a wafer for later use by using a punching machine after the sample is dried; and assembled into a CR2032 button cell in a glove box.
The invention has the beneficial effects that:
(1) the invention adopts a self-template method, does not need a template removing step, and has simple method and easy control of the appearance. The sample still keeps a relatively complete nano flower-like structure after high-temperature vulcanization, and has relatively good structural stability.
(2) The method has the advantages of mild reaction conditions, safe and easily-operated process, high yield and high repetition rate.
(1) The nanoflower structure contains a gap structure, and the carbon material is compounded with the nanoflower structure, so that stress change can be effectively relieved, structural damage in the charging and discharging process is reduced, and excellent electrochemical performance is obtained.
Drawings
FIG. 1 is an SEM image of a sample of a glycerol metal complex of example 1;
FIG. 2 is an SEM image of a solvothermal sample of specific example 1;
FIG. 3 is an SEM image of a carbon-coated transition metal sulfide sample of specific example 1;
FIG. 4 is a graph of electrochemical cycling performance of a carbon-coated transition metal sulfide sample as a negative electrode material of a lithium ion battery at a current density of 5A/g in example 1.
Detailed Description
The invention will be further illustrated with reference to specific embodiments and the accompanying drawings.
Example 1
Step 1: 0.1g of nickel nitrate and 0.1g of cobalt nitrate were weighed into 80mL of a mixed solvent of glycerin and isopropanol in a volume ratio of 1: and 3, magnetically stirring until the metal complex is completely dissolved, transferring the mixture into a reaction kettle, reacting for 4 hours at 160 ℃, naturally cooling to room temperature, washing with alcohol, centrifuging, and drying to obtain the glycerol metal complex sample.
Step 2: a 0.08g sample of a glycerol metal complex was weighed into 150mL of a mixed solvent of ethanol and water in a volume ratio of ethanol to water of 1: and (3) carrying out ultrasonic treatment for 10min at 0.5, transferring the mixture into a reaction kettle, reacting for 6h at 100 ℃, naturally cooling to room temperature, and carrying out water washing, alcohol washing, centrifugation and drying to obtain a solvothermal sample.
And step 3: weighing 0.1g of solvothermal sample, 0.05g of dopamine hydrochloride and 0.06g of tris (hydroxymethyl) aminomethane into 80mL of water, stirring and reacting for 6 hours at room temperature, and washing with water, washing with alcohol, centrifuging and drying to obtain a polydopamine-coated sample.
And 4, step 4: uniformly mixing 0.05g of polydopamine-coated sample and 0.15g of sulfur powder, transferring the mixture into a ceramic square boat, carrying out vulcanization treatment in a tube furnace under the protection of argon, preserving heat for 4h at 250 ℃, and taking out the sample after the vulcanization treatment is finished under the protection of inert gas until the sample is naturally cooled to obtain the carbon-coated transition metal sulfide material.
Example 2
Step 1: 0.16g of nickel chloride and 0.24g of cobalt chloride were weighed into 80mL of a mixed solvent of glycerin and isopropanol in a volume ratio of 1: and 4, magnetically stirring until the metal complex is completely dissolved, transferring the mixture into a reaction kettle, reacting for 6 hours at 170 ℃, naturally cooling to room temperature, washing with alcohol, centrifuging, and drying to obtain a glycerol metal complex sample.
Step 2: a 0.16g sample of a glycerol metal complex was weighed into 150mL of a mixed solvent of ethanol and water in a volume ratio of ethanol to water of 1: and 1, performing ultrasonic treatment for 20min, transferring the mixture into a reaction kettle, reacting for 10h at 120 ℃, naturally cooling to room temperature, and performing water washing, alcohol washing, centrifugation and drying to obtain a solvothermal sample.
And step 3: weighing 0.15g of solvothermal sample, 0.08g of dopamine hydrochloride and 0.08g of tris (hydroxymethyl) aminomethane into 100mL of water, stirring and reacting for 8 hours at room temperature, and washing with water, washing with alcohol, centrifuging and drying to obtain a polydopamine-coated sample.
And 4, step 4: uniformly mixing 0.05g of polydopamine-coated sample and 0.25g of sulfur powder, transferring the mixture into a ceramic square boat, carrying out vulcanization treatment in a tube furnace under the protection of argon, keeping the temperature at 300 ℃ for 6h, and taking out the sample after the vulcanization treatment is finished under the protection of inert gas until the sample is naturally cooled to obtain the carbon-coated transition metal sulfide material.
Example 3
Step 1: 0.2g of nickel acetate and 0.4g of cobalt acetate were weighed into 80mL of a mixed solvent of glycerin and isopropanol in a volume ratio of 1: and 5, magnetically stirring until the metal complex is completely dissolved, transferring the mixture into a reaction kettle, reacting for 8 hours at 180 ℃, naturally cooling to room temperature, washing with alcohol, centrifuging, and drying to obtain a glycerol metal complex sample.
Step 2: a 0.24g sample of a glycerol metal complex was weighed into 150mL of a mixed solvent of ethanol and water in a volume ratio of ethanol to water of 1: and 2, carrying out ultrasonic treatment for 25min, transferring the mixture into a reaction kettle, reacting for 15h at 140 ℃, naturally cooling to room temperature, and carrying out water washing, alcohol washing, centrifugation and drying to obtain a solvothermal sample.
And step 3: weighing 0.2g of solvothermal sample, 0.13g of dopamine hydrochloride and 0.1g of tris (hydroxymethyl) aminomethane into 120mL of water, stirring and reacting for 10 hours at room temperature, and washing with water, washing with alcohol, centrifuging and drying to obtain a polydopamine-coated sample.
And 4, step 4: uniformly mixing 0.05g of polydopamine-coated sample and 0.5g of sulfur powder, transferring the mixture into a ceramic square boat, carrying out vulcanization treatment in a tube furnace under the protection of argon, keeping the temperature at 400 ℃ for 8h, and taking out the sample after the vulcanization treatment is finished under the protection of inert gas until the sample is naturally cooled to obtain the carbon-coated transition metal sulfide material.
Example 4
Step 1: 0.8g of nickel nitrate was weighed into 80mL of a mixed solvent of glycerin and isopropanol in a volume ratio of 1: and 6, magnetically stirring until the metal complex is completely dissolved, transferring the mixture into a reaction kettle, reacting for 10 hours at 190 ℃, naturally cooling to room temperature, washing with alcohol, centrifuging, and drying to obtain the glycerol metal complex sample.
Step 2: weighing 0.3g of a glycerol metal complex sample in 150mL of a mixed solvent of ethanol and water, wherein the volume ratio of ethanol to water is 1: and 3, carrying out ultrasonic treatment for 30min, transferring the mixture into a reaction kettle, reacting for 15h at 140 ℃, naturally cooling to room temperature, washing with water, washing with alcohol, centrifuging, and drying to obtain a solvothermal sample.
And step 3: weighing 0.25g of solvothermal sample, 0.18g of dopamine hydrochloride and 0.12g of tris (hydroxymethyl) aminomethane into 140mL of water, stirring and reacting at room temperature for 12h, and washing with water, washing with alcohol, centrifuging and drying to obtain a polydopamine-coated sample.
And 4, step 4: uniformly mixing 0.05g of polydopamine-coated sample and 0.75g of sulfur powder, transferring the mixture into a ceramic square boat, carrying out vulcanization treatment in a tube furnace under the protection of argon, preserving heat for 10 hours at 500 ℃, and taking out the sample after the vulcanization treatment is finished under the protection of inert gas until the sample is naturally cooled to obtain the carbon-coated transition metal sulfide material.
Example 5
Step 1: weighing 1g of cobalt nitrate in 80mL of a mixed solvent of glycerol and isopropanol, wherein the volume ratio of the glycerol to the isopropanol is 1: and 7, magnetically stirring until the metal complex is completely dissolved, transferring the mixture into a reaction kettle, reacting for 12 hours at 200 ℃, naturally cooling to room temperature, washing with alcohol, centrifuging, and drying to obtain a glycerol metal complex sample.
Step 2: a 0.35g sample of a glycerol metal complex was weighed into 150mL of a mixed solvent of ethanol and water in a volume ratio of ethanol to water of 1: and 4, performing ultrasonic treatment for 30min, transferring the mixture into a reaction kettle, reacting for 24h at 180 ℃, naturally cooling to room temperature, and performing water washing, alcohol washing, centrifugation and drying to obtain a solvothermal sample.
And step 3: weighing 0.3g of solvothermal sample, 0.25g of dopamine hydrochloride and 0.15g of tris (hydroxymethyl) aminomethane into 160mL of water, stirring and reacting for 24 hours at room temperature, and washing with water, washing with alcohol, centrifuging and drying to obtain a polydopamine-coated sample.
And 4, step 4: uniformly mixing 0.05g of polydopamine-coated sample and 1g of sulfur powder, transferring the mixture into a ceramic square boat, carrying out vulcanization treatment in a tube furnace under the protection of argon, preserving heat for 12 hours at 600 ℃, and taking out the sample after the vulcanization treatment is finished under the protection of inert gas until the sample is naturally cooled to obtain the carbon-coated transition metal sulfide material.
The above-mentioned embodiments only express the embodiments of the present invention, but not should be understood as the limitation of the scope of the invention patent, it should be noted that, for those skilled in the art, many variations and modifications can be made without departing from the concept of the present invention, and these all fall into the protection scope of the present invention.
Claims (8)
1. A preparation method of a carbon-coated transition metal sulfide nanoflower structure is characterized by comprising the following steps:
firstly, adding metal salt into a mixed solvent of glycerol and isopropanol at room temperature, fully stirring until the metal salt is dissolved, transferring the mixture into a high-temperature high-pressure reaction kettle, reacting for 4-12h at the temperature of 160-200 ℃, and naturally cooling to room temperature, washing with alcohol, centrifuging and drying to obtain a glycerol metal complex sample;
secondly, adding a glycerol metal complex into a mixed solvent of water and ethanol, carrying out ultrasonic treatment for a period of time, transferring the mixture into a high-temperature high-pressure reaction kettle, reacting for 6-24h at the temperature of 100-180 ℃, and after naturally cooling to room temperature, carrying out water washing, alcohol washing, centrifugation and drying to obtain a solvothermal sample;
thirdly, adding the solvent thermal sample, dopamine hydrochloride and tris (hydroxymethyl) aminomethane into a proper amount of water, stirring and reacting for 6-24h at room temperature, and performing water washing, alcohol washing, centrifugation and drying to obtain a polydopamine coated sample; wherein, every 80-160mL of water is correspondingly added with: 0.1-0.3g of a solvothermal sample, 0.05-0.25g of dopamine hydrochloride, 0.06-0.15g of tris (hydroxymethyl) aminomethane;
and fourthly, mixing the polydopamine coated sample with sulfur powder, then carrying out vulcanization treatment in a tubular furnace under the protection of argon gas, carrying out vulcanization treatment at the temperature of 250-600 ℃ for 4-12h, and taking out the sample after the vulcanization treatment is finished under the protection of inert gas, and naturally cooling the sample to obtain the carbon-coated transition metal sulfide material.
2. The method of claim 1, wherein the metal salt in the first step is one of cobalt nitrate, nickel nitrate, cobalt acetate, nickel acetate, cobalt chloride, nickel chloride, and combinations thereof.
3. The method for preparing a carbon-coated transition metal sulfide nanoflower structure according to claim 1, wherein in the first step, 0.2-1g of metal salt is added to 80ml of mixed solvent, and the volume ratio of glycerol to isopropanol in the mixed solvent is 1: 3-1: 7.
4. the method of claim 1, wherein 0.08-0.5g of glycerol metal complex is added to 150mL of mixed solvent in the second step, wherein the volume ratio of ethanol to water in the mixed solvent is 1: 0.5-1: 4.
5. the method for preparing a carbon-coated transition metal sulfide nanoflower structure according to claim 1, wherein the ultrasonic time in the second step is 10-30 min.
6. The method for preparing a carbon-coated transition metal sulfide nanoflower structure according to claim 1, wherein the mass ratio of the polydopamine-coated sample to the sulfur powder in the fourth step is 1: 3-1: 20.
7. a carbon-coated transition metal sulfide nanoflower structure obtained by the preparation method according to any one of claims 1 to 6.
8. The use of the carbon-coated transition metal sulfide nanoflower structure of claim 7 as a negative active material for lithium ion batteries.
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