CN115196695A - Preparation method and application of nickel disulfide carbon-coated composite material - Google Patents

Preparation method and application of nickel disulfide carbon-coated composite material Download PDF

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CN115196695A
CN115196695A CN202210797695.5A CN202210797695A CN115196695A CN 115196695 A CN115196695 A CN 115196695A CN 202210797695 A CN202210797695 A CN 202210797695A CN 115196695 A CN115196695 A CN 115196695A
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nickel
solid
solution
composite material
carbon
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刘芝婷
吴泽南
崔钰燕
蔡建钟
郑文芝
范浩森
杨伟
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Guangzhou University
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Abstract

The invention relates to the technical field of a nickel disulfide carbon-coated composite material, and discloses a preparation method of a nickel disulfide carbon-coated composite material, which comprises the following steps: s1: synthesis of Ni (OH) (OCH) precursor containing Ni 3 ) (ii) a S2: the surface is coated with polydopamine; s3: synthesis of NiS 2 @ C, the final product is the nickel disulfide carbon-coated composite material spherical NiS 2 @ C solid. The invention also discloses application of the composite material in the manufacture of lithium ion batteries. The inventionAiming at some defects and limitations of common nickel disulfide, a novel structure is designed, partial problems of nickel disulfide as a battery cathode are solved, and the capacity and the service life of the battery are improved.

Description

Preparation method and application of nickel disulfide carbon-coated composite material
Technical Field
The invention relates to the technical field of nickel disulfide-coated carbon composite materials, in particular to a preparation method and application of a nickel disulfide-coated carbon composite material.
Background
In recent years, lithium Ion Batteries (LIBs) have become the primary energy source of choice for various portable electronic markets and electric transportation tool markets by virtue of their characteristics of high power density, high energy density, convenience, and the like. However, the lithium resource reserves in China are low, the distribution is unbalanced, and the lithium ion resources are further scarce and the price is increased in long-term large-scale application. Under the environment, sodium is taken as a family of lithium, the properties of the lithium and the family are relatively close, and the storage capacity of sodium in the earth is relatively high, so that Sodium Ion Batteries (SIBs) are promoted to have higher commercial application value, and the sodium ion batteries are expected to become a promising substitute of lithium ion batteries. However, the larger radius of sodium ions in sodium ion batteries leads to severe volume change during sodium desorption/insertion, so that most of the electrode materials of lithium ion batteries at present cannot be applied (resulting in lower battery capacity and cycle life). Therefore, it is still a very challenging research to make cathode materials for sodium ion batteries with high energy density and high cycling stability to achieve high performance of the batteries, and how to select the cathode materials is one of the main research issues of sodium ion batteries.
NiS2 has higher theoretical specific capacity (872 mAh/g), higher corrosion resistance and lower material processing cost, and compared with other sulfides, niS2 is more concerned by scientists. The conductivity of the electrode material affects the performance of the battery, and meanwhile, the material undergoes volume expansion in the operation process of the battery, and if the volume expansion is too large, the reaction discharge stability of the material is affected, so that the performance of the battery is affected. Since NiS2 has low conductivity and large volume change in the conversion reaction, its capacity retention or charge transfer capability is poor, and needs further optimization before being used as an excellent battery negative electrode material. Many attempts have been made to improve the reversible capacity, cycling stability and rate capability of NiS 2. For example, the coating is performed by using a carbonaceous material, the performance of the battery is improved by using the high conductivity of carbon, the volume and structure change of the nickel disulfide particles converted into metallic nickel in the discharging/charging process is buffered, and for the preparation of common NiS2 particles, the nickel-containing precursor is generally synthesized by calcining the preliminarily synthesized nickel-containing precursor with sublimed sulfur in a nitrogen atmosphere. The coating technology of the surface carbon layer is also applied to the synthesis process of other metal sulfides, for example, a nickel-containing precursor is prepared firstly, then a layer of Polydopamine (PDA) is coated on the surface, and then the NiS2 particles are obtained through further treatment (for example, calcination with sublimed sulfur in nitrogen) after the polydopamine is coated on the surface, the pure nickel disulfide is used as an electrode material, the performance is single, and factors influencing the performance cannot be overcome, and the factors easily cause poor performance of the battery, even cause the problems of capacity reduction, long service life reduction and the like. For example, the volume expansion of the material occurs during the operation of the battery, while the volume expansion of the sulfide is more serious, so that the volume expansion of the material during the reaction can be limited by using a layer of carbon skeleton. Meanwhile, the conductivity of the nickel disulfide is poor, and the excellent conductivity of the carbon material can be utilized, so that the overall conductivity of the electrode material is improved.
Disclosure of Invention
The invention aims to provide a preparation method and application of a nickel disulfide-coated carbon composite material, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a nickel disulfide carbon-coated composite material is characterized by comprising the following steps:
s1: synthesis of Ni (OH) (OCH) precursor containing Ni 3 )
Weighing a set amount of nickel acetate tetrahydrate, dissolving the nickel acetate tetrahydrate in 60mL of methanol, stirring the solution for a period of time under a magnetic stirrer until the nickel acetate tetrahydrate is fully dissolved to form a 0.01-0.03mol/L uniform solution, adding a set amount of CTAB (cetyl trimethyl ammonium bromide) into the solution, continuing stirring the solution until solids are fully dissolved, pouring the mixed solution into a 100mL reaction kettle, sealing the reaction kettle tightly, and putting the reaction kettle into a blast oven to perform hydrothermal reaction;
s2: surface coated polydopamine
Preparing 50mL of Tris (Tris-hydroxymethyl-aminomethane) solution with the concentration of 0.01mol/L and water as a solvent, respectively weighing 0.05g of nickel-containing precursor and 0.025g of dopamine hydrochloride, adding the weighed materials into the solution, and stirring the solution at room temperature for 24 hours;
s3: synthesis of NiS2@ C
Respectively weighing 0.05g of prepared Ni (OH) (OCH 3) @ PDA solid and 0.1g of sublimed sulfur (S), placing the solid and the sublimed sulfur (S) at two ends of a glass bottle, placing the glass bottle into a tubular furnace, heating to 350 ℃ at the heating rate of 2-6 ℃ min < -1 > under the protection of nitrogen, preserving the heat at 350-450 ℃ for 2 hours, and after the reaction is finished and the tubular furnace is cooled to the room temperature, obtaining the final product, namely the nickel disulfide carbon-coated composite NiS 2 @ C solid.
Preferably, 0.2986g of nickel acetate tetrahydrate is weighed out in S1 and stirred for 1 hour under a magnetic stirrer.
Preferably, 0.01-0.03g CTAB (cetyltrimethylammonium bromide) is added to the solution in S1, the oven is set at 180 ℃ and the reaction time is 48 hours.
Preferably, after the reaction in S1 is finished, the reaction kettle is taken out, the obtained mixed solution after the reaction is light green, then light green solid is obtained through suction filtration, organic polymer filter paper is used as the filter paper for suction filtration, the light green solid is washed twice by methanol and ethanol in the suction filtration process, and the solid obtained after suction filtration is dried in a vacuum oven at 80 ℃ for 12-20 hours to obtain the nickel-containing precursor with the particle size of about 2 microns.
Preferably, 50mL of water is measured in S2 by a measuring cylinder, the water is poured into a 100mL beaker, and then 0.06g of tris solid is weighed and dissolved in the water, and the solution is formed into a uniform solution by ultrasonic treatment in an ultrasonic cleaner for 20-60 minutes.
Preferably, dopamine hydrochloride in S2 can polymerize and form Polydopamine (PDA) nanofilm carbon spheres on almost any solid surface when exposed to air under weakly alkaline conditions (pH = 8.5).
Preferably, a tris solution is prepared in S2 to form a weak alkaline environment, and the obtained mixed solution is centrifugally washed to obtain a solid poly-dopamine-coated nickel-containing precursor (Ni (OH) (OCH) 3 ) @ PDA), after which the solid obtained is placed in a vacuum oven at 60 ℃ for 12 hours.
Preferably, in S3, a Poly Dopamine (PDA) layer on the surface of the nickel-containing precursor is carbonized, the nickel-containing precursor is vulcanized into NiS2 by controlling the temperature, a required spherical NiS2@ C solid is finally obtained, and meanwhile, the crystallinity of the NiS2 can be improved by calcining, and the conductivity of the NiS2 is improved.
Preferably, the spherical NiS2@ C solid prepared by the preparation method of any one of claims 1 to 8 is applied to a lithium ion battery material.
The preparation method and the application of the nickel disulfide carbon-coated composite material provided by the invention have the following beneficial effects:
(1) In the invention: the nickel disulfide-coated carbon composite material and the preparation method and application thereof design a novel structure aiming at some defects and limitations of common nickel disulfide, solve partial problems of nickel disulfide as a battery cathode, and improve the capacity and the service life of the battery;
(2) In the invention: the nickel disulfide-coated carbon composite material and the preparation method and the application thereof aim to prepare spherical nickel disulfide by utilizing a carbon sphere-coated synthesis scheme. The coating of carbon is utilized to increase the overall conductivity of the material, and simultaneously, the expansion phenomenon of the material in the operation process of the battery can be relieved;
(3) In the invention: when the nickel disulfide carbon-coated composite material is used as a negative electrode material of a sodium ion battery, the battery can reach high specific capacity of 412mAh g < -1 > under the current density of 0.1A g < -1 >.
Drawings
FIG. 1 is a schematic flow chart of the production process of the present invention;
FIG. 2 shows Ni (OH) (OCH) according to the present invention 3 ) A scanning electron microscope image;
FIG. 3 shows Ni (OH) (OCH) in accordance with the present invention 3 ) Scanning electron microscope images of II;
FIG. 4 shows the NiS of the present invention 2 Scanning electron microscope images of (a);
FIG. 5 shows NiS prepared by the present invention 2 Scanning electron micrographs of @ C;
FIG. 6 shows NiS prepared by the present invention 2 Rate performance plot of @ C;
FIG. 7 shows NiS prepared by the present invention 2 @ C cycle performance diagram.
Detailed Description
Example one
As shown in fig. 1 to 7, a method for preparing a nickel disulfide-coated carbon composite material provided by an embodiment of the present invention includes the following steps:
s1: synthesis of Ni (OH) (OCH) precursor containing Ni 3 ) Weighing 0.2986g of nickel acetate tetrahydrate in 60mL of methanol, stirring for 1 hour under a magnetic stirrer until the nickel acetate tetrahydrate is fully dissolved to form 0.01-0.03mol/L of uniform solution, adding 0.01-0.03g of CTAB (cetyl trimethyl ammonium bromide) into the solution, continuing stirring until the solid is fully dissolved, pouring the mixed solution into a 100mL reaction kettle, sealing, putting the reaction kettle into a forced air oven for hydrothermal reaction, setting the conditions of the oven at 180 ℃ for 48 hours, taking out the reaction kettle after the reaction is finished, taking out the obtained mixed solution after the reaction to be light green, then obtaining light green solid through suction filtration, using organic high polymer filter paper for suction filtration, respectively washing the light green solid twice by using methanol and ethanol in the suction filtration process, and drying the solid obtained after suction filtration in a vacuum oven at 80 ℃ for 12 hours to obtain a nickel-containing precursor with the particle size of about 2 mu m;
s2: the surface is coated with polydopamine, 50mL of Tris (Tris hydroxymethyl aminomethane) solution with the concentration of 0.01mol/L is prepared in S2, and the solvent is water. The specific operation is as follows: measuring 50mL of water by using a measuring cylinder, pouring the water into a 100mL beaker, then weighing 0.06g of tris solid, dissolving the tris solid in the water, carrying out ultrasound in an ultrasonic cleaner for 20-60 minutes to form a uniform solution, respectively weighing 0.05g of a nickel-containing precursor and 0.025g of dopamine hydrochloride, adding the solution into the solution, stirring the solution at room temperature for 24 hours, in the experiment, when the dopamine hydrochloride contacts air under a weak alkaline condition (pH = 8.5), polymerizing the dopamine hydrochloride on the surface of almost any solid to form a poly-dopamine (PDA) nano-film carbon sphere, preparing the tris solution to form a weak alkaline environment, carrying out centrifugal cleaning on the obtained mixed solution to obtain a solid poly-dopamine-coated nickel-containing precursor (Ni (OH) (OCH 3) @ PDA), and then placing the obtained solid in a vacuum oven at 60 ℃ for 12 hours;
s3: respectively weighing 0.05g of prepared Ni (OH) (OCH 3) @ PDA solid and 0.1g of sublimed sulfur (S) in the synthesized NiS2@ C and S3, placing the solid and the S at two ends of a glass bottle, then placing the glass bottle into a tube furnace, heating to 350 ℃ at the heating rate of 2-6 ℃ min < -1 > under the protection of nitrogen, preserving the temperature for 2 hours at 350-450 ℃, after the reaction is finished and the tube furnace is cooled to room temperature, obtaining the final product NiS2@ C, carbonizing a polydopamine layer (PDA) on the surface of a nickel-containing precursor in S3, simultaneously vulcanizing the nickel-containing precursor into NiS2 by controlling the temperature, and finally obtaining the required spherical NiS 2 The simultaneous calcination of the @ C solid can increase the crystallinity of NiS2 and increase NiS 2 The conductive performance of (1);
nickel disulfide carbon-coated composite spherical NiS prepared by adopting preparation method 2 The @ C solid is applied to the preparation of materials of lithium ion batteries.
Carry out two
As shown in fig. 1 to 7, the preparation method and application of the nickel disulfide-coated carbon composite material provided by the invention comprise the following steps:
s1: synthesis of Ni (OH) (OCH) precursor containing Ni 3 ) Weighing 0.2986g of nickel acetate tetrahydrate in S1, dissolving the nickel acetate tetrahydrate in 60mL of methanol, stirring the solution for 1 hour under a magnetic stirrer until the nickel acetate tetrahydrate is fully dissolved to form a 0.01-0.03mol/L uniform solution, adding 0.01-0.03g of CTAB (cetyl trimethyl ammonium bromide) into the solution, continuing stirring the solution until the solid is fully dissolved, pouring the mixed solution into a 100mL reaction kettle, sealing the reaction kettle tightly, putting the reaction kettle into a blast air oven to perform hydrothermal reaction, setting the conditions of the oven at 180 ℃, reacting for 48 hours, taking the reaction kettle out after the reaction is finished, obtaining a mixed solution after the reaction which is light green, then obtaining light green solid through suction filtration, wherein the suction filtration is carried out by using organic polymer filtrationWashing light green solids twice with methanol and ethanol respectively in the suction filtration process of paper, and drying the solids obtained after the suction filtration for 14 hours in a vacuum oven at 80 ℃ to obtain nickel-containing precursors with the particle size of about 2 mu m;
s2: the surface is coated with polydopamine, 50mL of Tris (Tris hydroxymethyl aminomethane) solution with the concentration of 0.01mol/L is prepared in S2, and the solvent is water. The specific operation is as follows: measuring 50mL of water by using a measuring cylinder, pouring the water into a 100mL beaker, then weighing 0.06g of tris solid, dissolving the tris solid in the water, carrying out ultrasound in an ultrasonic cleaner for 20-60 minutes to form a uniform solution, respectively weighing 0.05g of nickel-containing precursor and 0.025g of dopamine hydrochloride, adding the solution into the solution, stirring the solution at room temperature for 24 hours, in the experiment, when the dopamine hydrochloride contacts air under alkalescent conditions (pH = 8.5), polymerizing the dopamine hydrochloride on the surface of almost any solid to form poly-dopamine (PDA) nano thin-film carbon spheres, configuring tris solution to form an alkalescent environment, carrying out centrifugal cleaning on the obtained mixed solution to obtain a solid poly-dopamine-coated nickel-containing precursor (Ni (OH) (OCH 3) @ PDA), and then placing the obtained solid in a vacuum oven at 60 ℃ for 12 hours;
s3: 0.05g of prepared Ni (OH) (OCH) are respectively weighed in the synthesis of NiS2@ C, S3 3 ) @ PDA solid and 0.1g sublimed sulfur (S) are placed at two ends of a glass bottle, then the glass bottle is placed into a tube furnace, the temperature is raised to 350 ℃ at the heating rate of 2-6 ℃ min < -1 > under the protection of nitrogen, the temperature is kept at 350-450 ℃ for 2 hours, and after the reaction is finished and the tube furnace is cooled to the room temperature, the final product is NiS 2 @ C solid; s3, carbonizing a poly dopamine layer (PDA) on the surface of the nickel-containing precursor, and simultaneously vulcanizing the nickel-containing precursor into NiS2 by controlling the temperature to finally obtain the required spherical NiS 2 @ C solids, with co-calcination to enhance NiS 2 The crystallinity of the NiS2 is improved, and the conductivity of the NiS2 is improved;
nickel disulfide carbon-coated composite spherical NiS prepared by the preparation method 2 The @ C solid is applied to a lithium ion battery material and is used for preparing a lithium ion battery.
Implementation III
As shown in fig. 1 to 7, the preparation method and application of the nickel disulfide-coated carbon composite material provided by the invention comprise the following steps:
s1: synthesizing a nickel-containing precursor Ni (OH) (OCH 3), weighing 0.2986g of nickel acetate tetrahydrate in S1, dissolving the nickel acetate tetrahydrate in 60mL of methanol, stirring the solution for 1 hour under a magnetic stirrer until the nickel acetate tetrahydrate is fully dissolved to form a 0.01-0.03mol/L uniform solution, adding 0.01-0.03g of CTAB (hexadecyltrimethylammonium bromide) into the solution, continuing to stir until the solid is fully dissolved, pouring the mixed solution into a 100mL reaction kettle, sealing the reaction kettle tightly, putting the reaction kettle into a forced air oven to perform hydrothermal reaction, setting the conditions of the oven at 180 ℃, taking out the reaction kettle after the reaction is finished, obtaining a light green mixed solution after the reaction, then obtaining a light green solid by suction filtration, using organic high-molecular filter paper for the filter paper, respectively washing the light green solid twice with methanol and ethanol in the suction filtration process, and drying the solid obtained after the suction filtration in a vacuum oven at 80 ℃ for 16 hours to obtain the nickel-containing precursor with the particle size of about 2 mu m;
s2: the surface is coated with polydopamine, 50mL of Tris (Tris hydroxymethyl aminomethane) solution with the concentration of 0.01mol/L is prepared in S2, and the solvent is water. The specific operation is as follows: measuring 50mL of water by using a measuring cylinder, pouring the water into a 100mL beaker, then weighing 0.06g of tris solid, dissolving the tris solid in the water, carrying out ultrasound in an ultrasonic cleaner for 20-60 minutes to form a uniform solution, respectively weighing 0.05g of a nickel-containing precursor and 0.025g of dopamine hydrochloride, adding the solution into the solution, stirring the solution at room temperature for 24 hours, in the experiment, when the dopamine hydrochloride contacts air under a weak alkaline condition (pH = 8.5), polymerizing the dopamine hydrochloride on the surface of almost any solid to form a poly-dopamine (PDA) nano-film carbon sphere, preparing the tris solution to form a weak alkaline environment, carrying out centrifugal cleaning on the obtained mixed solution to obtain a solid poly-dopamine-coated nickel-containing precursor (Ni (OH) (OCH 3) @ PDA), and then placing the obtained solid in a vacuum oven at 60 ℃ for 12 hours;
s3: respectively weighing 0.05g of prepared Ni (OH) (OCH 3) @ PDA solid and 0.1g of sublimed sulfur (S) in the synthesized NiS2@ C and S3, placing the solid and the S at two ends of a glass bottle, then placing the glass bottle into a tubular furnace, heating to 350 ℃ at the heating rate of 2-6 ℃ min < -1 > under the protection of nitrogen, preserving the heat for 2 hours at 350-450 ℃, and after the reaction is finished and the tubular furnace is cooled to room temperature, carbonizing a polydopamine layer (PDA) on the surface of a nickel-containing precursor in the S3, and simultaneously vulcanizing the nickel-containing precursor into NiS2 by controlling the temperature to finally obtain the required spherical NiS2@ C solid, wherein the crystallinity of the NiS2 can be improved by calcining, and the conductivity of the NiS2 can be improved;
the application of the spherical NiS2@ C solid prepared by the preparation method of any one of claims 1-8 in lithium ion battery materials.
Practice four
As shown in fig. 1 to 7, the preparation method and application of the nickel disulfide-coated carbon composite material provided by the invention comprise the following steps:
s1: synthesizing a nickel-containing precursor Ni (OH) (OCH 3), weighing 0.2986g of nickel acetate tetrahydrate in S1, dissolving the nickel acetate tetrahydrate in 60mL of methanol, stirring for 1 hour under a magnetic stirrer until the nickel acetate tetrahydrate is fully dissolved to form a 0.01-0.03mol/L uniform solution, adding 0.01-0.03g of CTAB (cetyl trimethyl ammonium bromide) into the solution, continuously stirring until the solid is fully dissolved, pouring the mixed solution into a 100mL reaction kettle, sealing tightly, putting the reaction kettle into a forced air oven to perform hydrothermal reaction, setting the conditions of the oven at 180 ℃, reacting for 48 hours, taking out the reaction kettle after the reaction is finished, obtaining a light green mixed solution after the reaction, performing suction filtration to obtain a light green solid, using organic polymer filter paper as the filter paper, washing the light green solid twice with methanol and ethanol in the suction filtration process, and drying the solid obtained after the suction filtration in a vacuum oven at 80 ℃ for 20 hours to obtain a nickel-containing precursor with the particle size of about 2 mu m;
s2: the surface is coated with polydopamine, 50mL of Tris (Tris hydroxymethyl aminomethane) solution with the concentration of 0.01mol/L is prepared in S2, and the solvent is water. The specific operation is as follows: measuring 50mL of water by using a measuring cylinder, pouring the water into a 100mL beaker, then weighing 0.06g of tris solid, dissolving the tris solid in the water, carrying out ultrasound in an ultrasonic cleaner for 20-60 minutes to form a uniform solution, respectively weighing 0.05g of a nickel-containing precursor and 0.025g of dopamine hydrochloride, adding the solution into the solution, stirring the solution at room temperature for 24 hours, in the experiment, when the dopamine hydrochloride contacts air under a weak alkaline condition (pH = 8.5), polymerizing the dopamine hydrochloride on the surface of almost any solid to form a poly-dopamine (PDA) nano-film carbon sphere, preparing the tris solution to form a weak alkaline environment, carrying out centrifugal cleaning on the obtained mixed solution to obtain a solid poly-dopamine-coated nickel-containing precursor (Ni (OH) (OCH 3) @ PDA), and then placing the obtained solid in a vacuum oven at 60 ℃ for 12 hours;
s3: respectively weighing 0.05g of prepared Ni (OH) (OCH 3) @ PDA solid and 0.1g of sublimed sulfur (S) in the synthesized NiS2@ C and S3, placing the solid and the S at two ends of a glass bottle, then placing the glass bottle into a tubular furnace, heating to 350 ℃ at the heating rate of 2-6 ℃ min < -1 > under the protection of nitrogen, preserving the temperature for 2 hours at 350-450 ℃, and after the reaction is finished and the tubular furnace is cooled to room temperature, obtaining the final product NiS2@ C, carbonizing a polydopamine layer (PDA) on the surface of a nickel-containing precursor in the S3, and simultaneously vulcanizing the nickel-containing precursor into NiS2 by controlling the temperature, finally obtaining the required spherical NiS2@ C solid, and simultaneously calcining the solid to improve the crystallinity of the NiS2 and the conductivity of the NiS 2.
According to the embodiment of the invention, a novel structure is designed aiming at some defects and limitations of common nickel disulfide, so that part of problems of nickel disulfide as a battery cathode are solved, and the capacity and the service life of the battery are improved.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.

Claims (9)

1. A preparation method of a nickel disulfide carbon-coated composite material is characterized by comprising the following steps: which comprises the following steps:
s1: synthesis of Ni (OH) (OCH) precursor containing Ni 3 )
Weighing a set amount of nickel acetate tetrahydrate, dissolving the nickel acetate tetrahydrate in 60mL of methanol, stirring the solution for a period of time under a magnetic stirrer until the nickel acetate tetrahydrate is fully dissolved to form a 0.01-0.03mol/L uniform solution, adding a set amount of CTAB hexadecyl trimethyl ammonium bromide into the solution, continuing stirring the solution until solids are fully dissolved, pouring the mixed solution into a 100mL reaction kettle, sealing the reaction kettle tightly, and putting the reaction kettle into a blast oven to perform hydrothermal reaction;
s2: surface coated polydopamine
Preparing 50mL of Tris Tris (hydroxymethyl) aminomethane solution with the concentration of 0.01mol/L and water as a solvent, respectively weighing 0.05g of nickel-containing precursor and 0.025g of dopamine hydrochloride, adding the weighed materials into the solution, and stirring the solution at room temperature for 24 hours;
s3: synthesis of NiS 2 @C
0.05g of the prepared Ni (OH) (OCH) are weighed out separately 3 ) @ PDA solid and 0.1g sublimed sulfur were placed at both ends of a glass bottle, which was put in a tube furnace under nitrogen protection at 2-6 deg.C for min -1 The temperature rise rate is increased to 350 ℃, the temperature is kept at 350-450 ℃ for 2 hours, and after the reaction is finished and the tubular furnace is cooled to room temperature, the finally obtained product is the nickel disulfide carbon-coated composite material spherical NiS 2 @ C solid.
2. The method for preparing a nickel disulfide-carbon-coated composite material according to claim 1, wherein: in step S1, 0.2986g of nickel acetate tetrahydrate is weighed and stirred under a magnetic stirrer for 1 hour.
3. The method for preparing a nickel disulfide-carbon-coated composite material according to claim 2, wherein: and (3) adding 0.01-0.03g of CTAB into the solution in the step S1, setting the conditions of an oven at 180 ℃, and reacting for 48 hours.
4. The method for preparing a nickel disulfide-carbon-coated composite material according to claim 3, wherein: and (2) taking out the reaction kettle after the reaction in the step (S1) is finished, obtaining a light green mixed solution after the reaction, then obtaining a light green solid through suction filtration, wherein the filter paper obtained through suction filtration is organic high-molecular filter paper, washing the light green solid twice by using methanol and ethanol respectively in the suction filtration process, and drying the solid obtained through suction filtration in a vacuum oven at 80 ℃ for 12-20 hours to obtain a nickel-containing precursor with the particle size of about 2 microns.
5. The method for preparing a nickel disulfide-carbon-coated composite material according to claim 1, wherein: in the step S2, 50mL of water is measured by a measuring cylinder, poured into a 100mL beaker, and then 0.06g of tris (hydroxymethyl) aminomethane solid is weighed and dissolved in the water, and is subjected to ultrasonic treatment in an ultrasonic cleaner for 20-60 minutes to form a uniform solution.
6. The method for preparing a nickel disulfide-carbon-coated composite material according to claim 5, wherein: when dopamine hydrochloride contacts air under weak alkaline conditions (pH = 8.5) in step S2, it can polymerize and form Polydopamine (PDA) nanofilm carbon spheres on almost any solid surface.
7. The method for preparing a nickel disulfide-carbon-coated composite material according to claim 1, wherein: preparing a trihydroxymethyl aminomethane solution to form a weak alkaline environment in the step S2, and centrifugally cleaning the obtained mixed solution to obtain a solid polydopamine-coated nickel-containing precursor (Ni (OH) (OCH) 3 ) @ PDA), after which the solid obtained is placed in a vacuum oven at 60 ℃ for 12 hours.
8. The method for preparing a nickel disulfide-coated carbon composite material according to claim 7, wherein: step S3, carbonizing the poly dopamine layer PDA on the surface of the nickel-containing precursor, and simultaneously vulcanizing the nickel-containing precursor into NiS by controlling the temperature 2 Finally obtaining the required spherical NiS2@ C solid, and simultaneously calcining to improve the crystallinity of NiS2 and improve NiS 2 The conductive property of (3).
9. Nickel disulfide-coated carbon composite material, namely spherical NiS, prepared by the preparation method of any one of claims 1 to 8 2 Application of the @ C solid in the manufacture of lithium ion batteries.
CN202210797695.5A 2022-07-08 2022-07-08 Preparation method and application of nickel disulfide carbon-coated composite material Pending CN115196695A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012221855A (en) * 2011-04-12 2012-11-12 Sony Corp Positive electrode active material for nonaqueous electrolyte battery, positive electrode for nonaqueous electrolyte battery, and nonaqueous electrolyte battery, and battery pack, electronic device, electric vehicle, power storage device, and electric power system comprising nonaqueous electrolyte battery
CN108832097A (en) * 2018-06-13 2018-11-16 东华大学 A kind of curing nickel carbon nano-composite material and its preparation method and application
CN113314715A (en) * 2021-05-20 2021-08-27 广州大学 Nickel sulfide composite material and preparation method and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012221855A (en) * 2011-04-12 2012-11-12 Sony Corp Positive electrode active material for nonaqueous electrolyte battery, positive electrode for nonaqueous electrolyte battery, and nonaqueous electrolyte battery, and battery pack, electronic device, electric vehicle, power storage device, and electric power system comprising nonaqueous electrolyte battery
CN108832097A (en) * 2018-06-13 2018-11-16 东华大学 A kind of curing nickel carbon nano-composite material and its preparation method and application
CN113314715A (en) * 2021-05-20 2021-08-27 广州大学 Nickel sulfide composite material and preparation method and application thereof

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