CN113764623B - Nitrogen-carbon coated iron-nickel sulfide hollow composite material and preparation and application thereof - Google Patents

Nitrogen-carbon coated iron-nickel sulfide hollow composite material and preparation and application thereof Download PDF

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CN113764623B
CN113764623B CN202111001397.2A CN202111001397A CN113764623B CN 113764623 B CN113764623 B CN 113764623B CN 202111001397 A CN202111001397 A CN 202111001397A CN 113764623 B CN113764623 B CN 113764623B
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nickel sulfide
iron
nitrogen
composite material
nickel
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CN113764623A (en
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刘启明
陈鸿毅
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Douzhu Science And Technology Wuhan Co ltd
Wuhan University WHU
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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
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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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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Abstract

The invention discloses a nitrogen-carbon-coated iron-nickel sulfide hollow composite material and preparation and application thereof, wherein the composite material is characterized in that the surface of an iron-nickel sulfide hollow nanosphere is coated with a nitrogen-carbon shell layer, and the atomic ratio of iron to nickel to sulfur in the iron-nickel sulfide is (7); the diameter of the iron-nickel sulfide hollow nanosphere is 100-1000nm, and the thickness of the nitrogen-carbon shell layer is 5-10nm; the preparation method comprises the steps of adding ferrous sulfate heptahydrate and nickel sulfate hexahydrate into PVP/glycol solution, taking thiourea and sulfur powder as sulfur sources, carrying out hydrothermal synthesis, and carrying out solid solution and carbonization to obtain the product. The nitrogen-carbon coated iron-nickel sulfide hollow composite material provided by the invention is used as a negative electrode material of a sodium ion battery, and shows excellent cycling stability and higher specific capacity.

Description

Nitrogen-carbon coated iron-nickel sulfide hollow composite material and preparation and application thereof
Technical Field
The invention belongs to the field of nano composite materials, and particularly relates to a nitrogen-carbon coated iron-nickel sulfide hollow composite material as well as preparation and application thereof.
Background
The current severe ecological environment forces us to find more valuable energy storage methods, and the development of efficient energy conversion and storage technologies is more and more emphasized. The lithium ion battery is well known for large capacity and quick charging and has been successfully applied in the field of energy storage, but the further development of the lithium ion battery is limited by the lack and single distribution of lithium resources. Sodium resources are widely distributed on the earth, and sodium ion batteries and lithium ion batteries have the same 'rocking chair' charge and discharge principle. But Na + Radius ratio of (Li) + Large, making it more difficult to insert/de-insert in the lattice, which results in a rapid decay of the material's capacity. Therefore, a suitable electrode material is urgently required to solve this problem. The transition metal sulfide has high electrochemical activity and thermodynamic stability, and the metal-sulfur bond is weaker than the metal-oxygen bond, so thatHas received much attention as a negative electrode material for sodium ion batteries. Iron sulfide (FeS) is a typical metal sulfide with high theoretical specific capacity (609 mAhg) -1 ) Low cost, environment protection and rich resources. However, feS, a common defect of sulfide, has low intrinsic conductivity and inevitable volume expansion during charge and discharge, resulting in poor cycle performance and rate capability. Bimetallic sulfides have proven to be effective in improving cycling stability compared to monometallic sulfides. The strategy of the bimetal sulfide can establish an internal electric field and improve the conductivity.
CN109860593A discloses an iron-nickel sulfide, in the heat treatment process, under the co-catalysis of iron and nickel, a carbon nano tube coated particle structure is formed, and the iron-nickel sulfide is used as a negative electrode material of a sodium ion battery, so that the electrochemical sodium storage performance of the iron sulfide negative electrode material is obviously improved. CN110224126A discloses that a carbon nanotube grows from an iron-nickel sulfide nano material under the action of metal co-catalysis, the tubular structure of the carbon nanotube provides a buffer space for the volume expansion of iron-nickel sulfide generated in the charge-discharge process, the structural stability of the material is improved, and the carbon nanotube, as a sodium ion battery cathode material, can obviously improve the electrochemical sodium storage performance of an FeS cathode material. However, the specific capacity of the material used as the negative electrode material of the sodium-ion battery is still greatly different from the theoretical specific capacity of FeS.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a nitrogen-carbon coated iron-nickel sulfide hollow composite material, which is characterized in that the surface of an iron-nickel sulfide hollow nanosphere is coated with a nitrogen-carbon shell layer, and the atomic ratio of iron to nickel to sulfur in the iron-nickel sulfide is (7); the diameter of the iron-nickel sulfide hollow nanosphere is 100-1000nm, and the thickness of the nitrogen-carbon shell layer is 5-10nm. The nitrogen-carbon coated iron-nickel sulfide hollow composite material has high specific capacity and cycling stability.
The invention also provides a preparation method of the nitrogen-carbon coated iron-nickel sulfide hollow composite material, which comprises the following steps:
s1, mixing polyvinylpyrrolidone with ethylene glycol, and stirring for dissolving to obtain a PVP/ethylene glycol solution;
s2, adding ferrous sulfate heptahydrate and nickel sulfate hexahydrate into a PVP/ethylene glycol solution, stirring to dissolve, and adding thiourea and sulfur powder to obtain a mixed solution;
s3, pouring the mixed solution into a Teflon liner of a hydrothermal reaction kettle, reacting for 18 hours at 180 ℃, and centrifugally separating, washing and drying a reaction product to obtain black powder;
s4, placing the black powder into a porcelain boat, then placing the porcelain boat into a tubular furnace protected by argon atmosphere, reacting for 3h at 350 ℃, then heating to 600 ℃, reacting for 3h, and naturally cooling to obtain the nitrogen-carbon coated iron-nickel sulfide hollow composite material.
In the step S1, the weight average molecular weight of the polyvinylpyrrolidone is 58000, and the mass volume concentration of the PVP/ethylene glycol solution is 8-16 g/L.
In the step S2, the mass ratio of the ferrous sulfate heptahydrate, the nickel sulfate hexahydrate, the thiourea and the sulfur powder is 3.
And S3, washing the reaction product by sequentially adopting deionized water and absolute alcohol, and drying in a vacuum oven at the drying temperature of 60-100 ℃ for 12-24 h.
In step S4, the heating rate is 5 ℃/min.
The invention also provides application of the nitrogen-carbon coated iron-nickel sulfide hollow composite material in a sodium ion battery, and the nitrogen-carbon coated iron-nickel sulfide hollow composite material is used as a negative electrode material of the sodium ion battery.
The invention has the beneficial effects that: the hollow nanosphere structure of the nitrogen-carbon coated iron-nickel sulfide hollow composite material provides a buffer space for volume expansion generated by iron-nickel sulfide in the charging and discharging processes, and the nitrogen-carbon shell layer limits the expansion process, so that the expansion rate is reduced, and the structural stability of the material is improved; the lithium ion battery cathode material is applied to a sodium ion battery as a cathode material, shows excellent cycling stability and higher specific capacity, and is 0.2 A.g -1 Has a reversible capacity of 567.7 mAh g after 100 cycles at a current density of -1 The first turn coulombic efficiency was 88.52%; at 6 A.g -1 Can maintain 320mAh g even after 5000 cycles under the high current density -1 The capacity of (c).
Drawings
FIG. 1 is an HRTEM image of example 1 (a); (b) - (g) are the distribution diagrams of the elements.
FIG. 2 is SEM and TEM images of examples and comparative examples; the SEM pictures of (a), (b) and (c) are respectively example 1 and comparative examples 1 and 2; (d) The TEM images of example 1 and comparative examples 1 and 2 are shown in (e) and (f), respectively.
FIG. 3 shows the values of 0.2 A.g for example 1 -1 Cycling plot at current density.
FIG. 4 shows the results of example 1 and comparative examples 1 and 2 at 2A g -1 Cycle plot at current density.
FIG. 5 shows the results of example 1 at 6A. G -1 Cycle plot at current density.
Detailed Description
The technical solutions of the present invention will be described in detail and fully with reference to the following specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
Example 1
A nitrogen-carbon coated iron-nickel sulfide hollow composite material is prepared by the following steps:
s1, mixing 0.5g of polyvinylpyrrolidone (PVP, mw = 58000) with 50mL of glycol, stirring and dissolving to obtain a PVP/glycol solution;
s2, adding 3mmol of ferrous sulfate heptahydrate and 1mmol of nickel sulfate hexahydrate into a PVP/glycol solution, stirring for dissolving, and adding 4mmol of thiourea and 3mmol of sulfur powder to obtain a mixed solution;
s3, pouring the mixed solution into a Teflon liner of a hydrothermal reaction kettle, reacting for 18h at 180 ℃, centrifugally separating a reaction product, washing with deionized water and absolute alcohol in sequence, and drying in a vacuum oven at 60 ℃ for 24h to obtain black powder;
and S4, placing the black powder into a porcelain boat, then placing the porcelain boat into a tubular furnace protected by argon atmosphere, reacting for 3h at 350 ℃, then heating to 600 ℃ and reacting for 3h, wherein the heating rate is 5 ℃/min, and naturally cooling to obtain the nitrogen-carbon coated iron-nickel sulfide hollow composite material.
In the hollow composite material of iron-nickel sulfide coated with nitrogen and carbon prepared in this example, the atomic ratio of iron to nickel to sulfur is 7; as shown in FIGS. 1 and 2, the hollow nanospheres have a diameter of 100-1000nm and a nitrogen-carbon shell of 5-10nm.
Table 1 example 1 element content
Element Atom/(EDS) Atom/(ICP)
Fe 33.2％ 32％
Ni 14.2％ 13.2％
S 52.6％ 54.8％
Comparative example 1
A nitrogen-carbon coated iron-nickel sulfide hollow composite material is prepared by the following steps:
s1, mixing 0.5g of polyvinylpyrrolidone (PVP, mw = 58000) with 50mL of glycol, stirring and dissolving to obtain a PVP/glycol solution;
s2, adding 2mmol of ferrous sulfate heptahydrate and 2mmol of nickel sulfate hexahydrate into a PVP/glycol solution, stirring for dissolving, and adding 4mmol of thiourea and 3mmol of sulfur powder to obtain a mixed solution;
s3, pouring the mixed solution into a Teflon inner container of a hydrothermal reaction kettle, reacting for 18 hours at 180 ℃, centrifugally separating a reaction product, washing the reaction product by using deionized water and absolute ethyl alcohol in sequence, and drying the reaction product in a vacuum oven at the drying temperature of 60 ℃ for 24 hours to obtain black powder;
and S4, placing the black powder into a porcelain boat, then placing the porcelain boat into a tubular furnace protected by argon atmosphere, reacting for 3h at 350 ℃, then heating to 600 ℃ and reacting for 3h, wherein the heating rate is 5 ℃/min, and naturally cooling to obtain the nitrogen-carbon coated iron-nickel sulfide hollow composite material.
The atomic ratio of iron, nickel and sulfur in the hollow composite material of the nitrogen-carbon coated iron-nickel sulfide prepared by the comparative example is 3; as shown in FIG. 2, the diameter of the hollow nanosphere is 100-1000nm and the thickness of the nitrogen-carbon shell is 5-10nm.
Table 2 comparative example 1 element content
Element Atom/(EDS) Atom/(ICP)
Fe 14.3％ 18.1％
Ni 33％ 27％
S 52.7％ 54.9％
Comparative example 2
A nitrogen-carbon coated iron-nickel sulfide hollow composite material is prepared by the following steps:
s1, mixing 0.5g of polyvinylpyrrolidone (PVP, mw = 58000) with 50mL of glycol, stirring and dissolving to obtain a PVP/glycol solution;
s2, adding 1mmol of ferrous sulfate heptahydrate and 3mmol of nickel sulfate hexahydrate into the PVP/glycol solution, stirring for dissolving, and adding 4mmol of thiourea and 3mmol of sulfur powder to obtain a mixed solution;
s3, pouring the mixed solution into a Teflon liner of a hydrothermal reaction kettle, reacting for 18h at 180 ℃, centrifugally separating a reaction product, washing with deionized water and absolute alcohol in sequence, and drying in a vacuum oven at 60 ℃ for 24h to obtain black powder;
and S4, placing the black powder into a porcelain boat, then placing the porcelain boat into a tubular furnace protected by argon atmosphere, reacting for 3h at 350 ℃, then heating to 600 ℃ and reacting for 3h, wherein the heating rate is 5 ℃/min, and naturally cooling to obtain the nitrogen-carbon coated iron-nickel sulfide hollow composite material.
The atomic ratio of iron, nickel and sulfur in the hollow composite material of the nitrogen-carbon coated iron-nickel sulfide prepared by the comparative example is 1; as shown in FIG. 2, the diameter of the hollow nanosphere is 100-1000nm and the thickness of the nitrogen-carbon shell is 5-10nm.
Table 3 content of elements of comparative example 2
Element Atom/(EDS) Atom/(ICP)
Fe 6％ 6.5％
Ni 42.6％ 38.2％
S 51.4％ 55.3％
The nitrogen-carbon coated iron-nickel sulfide hollow composite materials prepared in the above examples and comparative examples were used as a negative electrode of a sodium ion battery, and electrochemical properties thereof were tested by a constant current charge-discharge technique using a blue cell test system.
FIG. 3 shows the values of 0.2 A.g for example 1 -1 The cycle chart under the current density shows that the specific capacity is kept at 567mAh g after 100 cycles of cycle -1 。
FIG. 4 shows the results of example 1 and comparative examples 1 and 2 at 2A g -1 The cycle diagram under the current density shows that after 900 cycles, the specific capacity of the sample 1 is kept to 477mAh g < -1 >, and the specific capacity of the comparative sample 1 is kept to 367mAh g -1 Comparative example 2 has a specific capacity of only 284mAh g -1 。
FIG. 5 shows the results of example 1 at 6A. G -1 The circulation diagram under the current density shows that the specific capacity is kept 320 mAh.g after 5000 cycles of circulation -1 。
Therefore, the nitrogen-carbon coated iron-nickel sulfide hollow composite material provided by the invention is used as a negative electrode material of a sodium ion battery, and has excellent cycling stability and higher specific capacity.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention disclosed herein are included in the scope of the present invention, and the scope of the present invention is subject to the scope of the claims.

Claims (8)

1. The preparation method of the nitrogen-carbon coated iron-nickel sulfide hollow composite material is characterized by comprising the following steps of:
s1, mixing polyvinylpyrrolidone with ethylene glycol, and stirring for dissolving to obtain a PVP/ethylene glycol solution;
s2, adding ferrous sulfate heptahydrate and nickel sulfate hexahydrate into a PVP/glycol solution, stirring to dissolve, and adding thiourea and sulfur powder to obtain a mixed solution;
s3, pouring the mixed solution into a Teflon liner of a hydrothermal reaction kettle, reacting for 18h at 180 ℃, and centrifugally separating, washing and drying a reaction product to obtain black powder;
s4, placing the black powder into a porcelain boat, then placing the porcelain boat into a tubular furnace protected by argon atmosphere, reacting for 3h at 350 ℃, then heating to 600 ℃, reacting for 3h, and naturally cooling to obtain the nitrogen-carbon coated iron-nickel sulfide hollow composite material.
2. The method for preparing the nitrogen-carbon coated iron-nickel sulfide hollow composite material according to claim 1, wherein the weight average molecular weight of the polyvinylpyrrolidone in the step S1 is 58000, and the mass volume concentration of the PVP/glycol solution is 8-16 g/L.
3. The method for preparing the nitrogen-carbon coated iron-nickel sulfide hollow composite material according to claim 1, wherein the mass ratio of the ferrous sulfate heptahydrate, the nickel sulfate hexahydrate, the thiourea and the sulfur powder in the step S2 is 3.
4. The method for preparing the hollow composite material of iron-nickel sulfide coated with nitrogen and carbon according to claim 1, wherein the reaction product is washed by deionized water and absolute alcohol in sequence in step S3, and then dried in a vacuum oven at 60-100 ℃ for 12-24 h.
5. The method for preparing the nitrogen-carbon coated iron-nickel sulfide hollow composite material according to claim 1, wherein the temperature rise rate in the step S4 is 5 ℃/min.
6. The nitrocarbon-coated iron-nickel sulfide hollow composite material prepared by the preparation method of any one of claims 1 to 5 is characterized in that the surface of the iron-nickel sulfide hollow nanosphere is coated with a nitrocarbon shell layer, and the atomic ratio of iron to nickel to sulfur in the iron-nickel sulfide is (7).
7. The nitrocarbon coated iron-nickel sulfide hollow composite material according to claim 6, wherein the diameter of the iron-nickel sulfide hollow nanospheres is 100-1000nm, and the thickness of the nitrocarbon shell layer is 5-10nm.
8. Use of the nitrogen-carbon coated iron-nickel sulfide hollow composite material prepared by the preparation method of any one of claims 1 to 5 or according to claim 6 or 7 as a negative electrode material of a sodium-ion battery.
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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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