CN108565429B - NaFeS as negative electrode material of sodium-ion battery2Preparation method of/C composite material - Google Patents
NaFeS as negative electrode material of sodium-ion battery2Preparation method of/C composite material Download PDFInfo
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Abstract
The invention relates to a sodium ion battery cathode material NaFeS2A preparation method of the/C composite material. The method comprises the following steps: taking a sodium-sulfur source, an iron source and a carbon source according to a proportion, uniformly mixing, and adding absolute ethyl alcohol to prepare slurry; drying after ball milling, and grinding again to obtain a precursor; under the protection of nitrogen atmosphere, the precursor is subjected to two-stage heating treatment to obtain NaFeS2a/C composite material. The method is carried out by solid phase carbothermic reduction heat treatment to change a carbon source into a carbon skeleton and NaFeS2The conductive material is attached to a carbon skeleton, so that the transmission of sodium ions is facilitated and the conductivity is increased; low cost, simple preparation process, and superior performance to FeS when used as the cathode material of sodium ion battery2A material.
Description
Technical Field
The invention relates to a sodium ion battery cathode material NaFeS2A preparation method of a/C composite material belongs to the technical field of negative electrode materials of sodium-ion batteries.
Background
The lithium ion battery has the advantages of large energy density, long cycle life, high working voltage, no memory effect, small natural discharge, wide working temperature range and the like. And along with lithium ion battery is applied to electric automobile gradually, the demand of lithium will greatly increased, and the reserves of lithium are limited, and distribute unevenly, this is a bottleneck problem to the development requires that the smart power grids of low price, security is high and renewable resources large-scale energy storage limit long-life energy storage battery. Therefore, there is a need to develop a new system of energy storage battery with excellent comprehensive performance, and sodium storage is very abundant and widely distributed compared with lithium resources. Metallic sodium and metallic lithium have similar chemical properties, and sodium ion batteries and lithium ion batteries also have similar charge and discharge principles. However, the radius of sodium ions is large compared with that of lithium ions, so that the sodium ions are difficult to be inserted into/extracted from the electrode material, and the electrochemical performance is poor. Therefore, the search for suitable electrode materials has become a key point in the development of sodium ion batteries.
FeS of pyrite type2The material has the advantages of rich resources, low price, no toxicity, high theoretical capacity and the like, is a sodium-ion battery electrode material with great application prospect, and attracts the wide attention and research of people. However, since FeS2Semiconductor properties and intercalation due to sodium ions during charging and dischargingThe insertion/extraction causes the collapse of the material structure, resulting in FeS2The capacity of the negative electrode material of the sodium-ion battery is quickly attenuated, and the rate capability is poor. And FeS2the/C utilizes the tiny particle size and the flexibility of carbon to weaken the stress change caused by the volume effect generated by the extraction and the embedding of the active substance, thereby weakening the pulverization of the electrode material and enhancing the cycle performance. With Fe (NO)3)3And CH3CSNH2Synthesizing micron-scale FeS serving as raw material by using hydrothermal method2The material is used as the negative electrode material of the sodium ion battery and is 100mA g-1The first discharge capacity is 718mAhg at the current density of (A)-1At a current density of 5000mAg-1In addition, 323mAh g can be maintained-1See Kongyao Chen et al, Mechanism of Capacity Fade in Sodium Storage and the Strategies of improvements for FeS2Enode, ACS appl.mater.interfaces 9(2017) 1536-1541; but the FeS synthesized by the method2The material is micron-sized, has larger grain diameter and FeS in the charge-discharge process2The material structure is prone to collapse. Patent document CN107452951A discloses a preparation of FeS by solvothermal method2Nano material and its application in negative pole of sodium ion battery. The method is carried out by reacting FeSe2Coating on FeS2The core-shell microsphere electrode material is formed on the material, and when the material is used as a negative electrode of a sodium ion battery, the thickness of the material is 100mAg-1The first discharge capacity is 600mAh g-1. As can be seen from the above prior art data, FeS2As a negative electrode material, the electrochemical performance is general.
NaFeS has not been found in natural environment2This material, which is a mixed-valence material, has chemical and physical properties that depend primarily on the oxidation state of iron. Wuhuaqiang et al reported a microwave-assisted method for preparing fibrous NaFeS2Nanoparticles, see spectroscopic and spectroscopic analysis, Vol.25, No. 6, 6.2005. However, so far, no NaFeS has been found2It is reported as a negative electrode material.
Disclosure of Invention
Aiming at the defects of the prior art, the technical task of the invention is to provide a methodNovel cathode material NaFeS of sodium ion battery2The invention also provides NaFeS with excellent electrochemical performance2A preparation method of the/C composite material.
The method adopts a solid phase method, uniformly mixes and grinds a sodium source, an iron source, a sulfur source and a carbon source, and synthesizes NaFeS through high-temperature calcination2and/C, the cathode material is used for the sodium ion battery.
The technical scheme of the invention is as follows:
NaFeS2The preparation method of the/C composite material comprises the following steps:
(1) according to the molar ratio of Na to Fe to S to C being 1:1:2: 3-6, taking a sodium-sulfur source, an iron source and a carbon source, uniformly mixing, and adding a proper amount of absolute ethyl alcohol to prepare slurry;
(2) putting the slurry obtained in the step (1) into a ball milling tank, and performing ball milling at 1000-1800 r min-1Grinding for 80-150 min at the rotating speed
Then drying at 50-60 ℃, and then grinding into powder to obtain a precursor;
(3) heating the precursor in the step (2) to 260-400 ℃ under the protection of nitrogen atmosphere, preserving heat for 100-300 min, continuously heating to 550-800 ℃, preserving heat for 300-600 min, and naturally cooling to room temperature to obtain NaFeS2a/C composite material.
In the step (3), the precursor is subjected to solid-phase carbothermic reduction heat treatment to change a carbon source into a carbon skeleton, and NaFeS is added2Attached to the carbon skeleton, which facilitates sodium ion transport and increases electrical conductivity.
Preferably according to the invention, in step (1), the sodium-sulfur source is sodium thiosulfate or sodium sulfide, preferably sodium thiosulfate;
preferably, in step (1), the iron source is ferrous oxalate, ferrous chloride or ferric chloride, preferably ferrous oxalate;
preferably, in step (1), the carbon source is sodium lignosulfonate, glucose or sucrose, preferably sucrose;
preferably, in step (1), the ratio of Na: Fe: S: C ═ 1:1:2: 3.5-5.5 mol ratio; most preferably, Na: Fe: S: C ═ 1:1:2: 4.2-4.6 mol ratio.
According to a preferred embodiment of the invention, in step (2), the number of grinding revolutions is 1200 rpm-1The grinding time is 100 min.
According to the invention, in the step (3), the heat treatment temperature is 300 ℃ and the holding time is 200min and 600 ℃ and the holding time is 480 min.
The most preferred embodiment of the present invention is the embodiment described in example 1.
Novel negative electrode material NaFeS of sodium ion battery prepared according to method2a/C composite material.
NaFeS prepared by the invention2The application of the/C composite material as a negative electrode material of a sodium-ion battery. The specific application method is as follows:
firstly, NaFeS is put into2Fully grinding and uniformly mixing the conductive agent and the binder with the/C, adding an N-methyl pyrrolidone solvent, and uniformly stirring to obtain pre-coating slurry;
coating the precoating slurry on a copper foil, drying the electrode plate to obtain the negative electrode plate of the sodium-ion battery, and using the obtained negative electrode plate of the sodium-ion battery for the sodium-ion battery of the button type battery.
The above-mentioned conductive agents and binders can be used according to the prior art, for example acetylene black and polyvinylidene fluoride.
The composite cathode material NaFeS of the sodium-ion battery prepared by the method of the invention2a/C, at a charging and discharging voltage of 0.01-3.0V and 1A g-1The first discharge specific capacity under the current is 1156.07mA hg-1And the specific discharge capacity exceeds the theoretical specific capacity and is 507.43mAh g after being cycled for 50 times-1。
The invention has the following beneficial effects:
the invention mixes and ball-mills a sodium source, a sulfur source, an iron source and a carbon source according to a proportion, and changes the carbon source into a carbon skeleton through solid-phase carbothermic reduction heat treatment, and NaFeS2Attached to a carbon skeleton, which facilitates the transport of sodium ions and increases conductivity; in addition, NaFeS2The sodium ions in the structure are distributed between Fe-S tetrahedron and shared tetrahedron, and when the structure is used as the electrode material of sodium ion battery, the sodium ionsThe seed can be embedded/separated better, and the structure is stable; and the carbon coating can effectively reduce the dissolution of sulfide in organic electrolyte and reduce the formation of an insulating layer of polysulfide outside an electrode, thereby effectively improving the charge-discharge capacity and the cycle performance of the material.
The invention synthesizes NaFeS by a simple and easy solid phase method2the/C composite material has low cost and simple preparation process, and has better performance than FeS when used as the cathode material of the sodium-ion battery2The material has good application prospect.
Drawings
FIG. 1 is NaFeS prepared in example 12XRD pattern of the/C composite material, wherein the ordinate represents intensity and the abscissa represents diffraction angle (2 theta).
FIG. 2 is NaFeS prepared in example 12EDS analysis of the/C composite.
FIG. 3 is NaFeS prepared in example 12And the electrochemical cycle performance of the/C composite material is shown.
Detailed Description
The present invention will be further described with reference to the following detailed description of embodiments thereof, but not limited thereto, in conjunction with the accompanying drawings.
The raw materials used in the examples are all commercially available raw materials.
Example 1 molar ratio of Na: Fe: S: C ═ 1:1:2:4.4
Mixing 2.482g of sodium thiosulfate, 1.799g of ferrous oxalate and 0.685g of sucrose, adding absolute ethyl alcohol to submerge the solid powder, stirring, putting into a ball milling tank, and performing 1200r min-1Grinding for 100min at the rotating speed of (1) to obtain a paste mixture; drying the precursor at 60 ℃, and grinding the dried precursor into powder to obtain a precursor; finally heating the NaFeS to 300 ℃ in nitrogen atmosphere, preserving heat for 200min, then continuously heating to 600 ℃ and preserving heat for 480min, and naturally cooling to obtain NaFeS2a/C composite material. Prepared NaFeS2The XRD pattern and EDS analysis pattern of the/C nano composite material are shown in figure 1 and figure 2. From the XRD pattern of FIG. 1, the main diffraction peak and NaFeS of the synthesized product can be seen2Standard cards of crystalline phases correspond, and no other crystalline phases; from the EDS analysis chart of FIG. 2, it can be seen that the main chemical components of the synthesized productIs Na, Fe, S and C, so the synthesized product is NaFeS2a/C composite material, wherein C is an amorphous phase.
Electrochemical performance test
NaFeS obtained in example 1 was added2the/C composite material is used for a sodium ion battery, and an electrode is prepared by adopting a coating method. Adding NaFeS2Fully grinding and mixing the acetylene black and polyvinylidene fluoride (PVDF) according to the mass ratio of 8:1:1, adding an N-methyl pyrrolidone solvent, uniformly stirring to obtain pre-coated refined slurry, coating the pre-coated refined slurry on a copper foil, drying at 60 ℃ for 6 hours and vacuum drying at 120 ℃ for 12 hours, naturally cooling, and cutting into a wafer with the diameter of 15mm by using a punching machine to obtain the negative electrode plate of the sodium ion battery. Sequentially assembling the positive electrode shell, the electrode plate, the electrolyte, the diaphragm, the electrolyte, the lithium plate, the gasket and the negative electrode shell, and sealing the battery by using a sealing machine to obtain the CR2032 type button half-battery. And finally, performing constant-current charge and discharge test on the battery by an A713-2008S-3TGF-A type high-precision charge and discharge instrument.
NaFeS prepared as above using example 12The first discharge specific capacity of the/C negative electrode material is 1156mAh g under the conditions that the charge-discharge voltage is 0.01-3.00V and the current density is 1000mA/g-1And the discharge capacity after 50 times of circulation is 507mAhg-1As shown in fig. 3.
Example 2 Na: Fe: S: C ═ 1:1:2:3.5 molar ratio
Adding 4.604g sodium sulfide, 1.988g ferrous chloride, and 1.149g glucose into anhydrous ethanol to immerse the solid powder, mixing, placing into a non-ball-milling tank, and standing at 1800r min-1Grinding for 80min at the rotating speed of (1) to obtain a paste mixture; drying the precursor at 60 ℃, and grinding the dried precursor into powder to obtain a precursor; finally, heating the NaFeS to 260 ℃ in nitrogen atmosphere, preserving heat for 300min, then continuously heating to 800 ℃ and preserving heat for 300min, and naturally cooling to obtain NaFeS2a/C composite material. When the material is used as a negative electrode material of a sodium-ion battery, the first discharge specific capacity is 852mAh g under the conditions that the voltage is 0.01-3.00V and the current density is 1000mA/g-1And the discharge capacity after 50 times of circulation is 327mAh g-1。
Example 3 Na: Fe: S: C ═ 1:1:2:5.5 molar ratio
Adding 2.482g sodium thiosulfate, 2.703g ferric chloride and 1.470g sodium lignosulfonate into anhydrous ethanol to immerse the solid powder, mixing, placing into a non-ball-milling tank, and standing for 1000r min-1Grinding for 150min at the rotating speed of (1) to obtain a paste mixture; drying the precursor at 60 ℃, and grinding the dried precursor into powder to obtain a precursor; finally heating the NaFeS to 400 ℃ in nitrogen atmosphere, preserving heat for 100min, then continuously heating to 550 ℃ and preserving heat for 600min, and naturally cooling to obtain NaFeS2a/C composite material. When the material is used as a negative electrode material of a sodium-ion battery, the first specific discharge capacity is 747mAh g under the conditions that the voltage is 0.01-3.00V and the current density is 1000mA/g-1And the discharge capacity after 50 times of circulation is 442mAh g-1。
Claims (11)
1. NaFeS2The preparation method of the/C composite material comprises the following steps:
(1) according to the mol ratio of Na to Fe to S to C =1: 1:2: 3-6, taking a sodium-sulfur source, an iron source and a carbon source, uniformly mixing, and adding a proper amount of absolute ethyl alcohol to prepare slurry;
(2) putting the slurry obtained in the step (1) into a ball milling tank, and performing ball milling at 1000-1800 r min-1Grinding for 80-150 min at the rotating speed, drying at 50-60 ℃, and grinding into powder to obtain a precursor;
(3) heating the precursor in the step (2) to 260-400 ℃ under the protection of nitrogen atmosphere, preserving heat for 100-300 min, continuously heating to 550-800 ℃, preserving heat for 300-600 min, and naturally cooling to room temperature to obtain NaFeS2a/C composite material.
2. NaFeS as claimed in claim 12The preparation method of the/C composite material is characterized in that in the step (1), the sodium-sulfur source is sodium thiosulfate or sodium sulfide.
3. NaFeS as claimed in claim 12The preparation method of the/C composite material is characterized in that in the step (1), the iron source is ferrous oxalate, ferrous chloride or ferric chloride.
4. As claimed inNaFeS as defined in claim 12The preparation method of the/C composite material is characterized in that in the step (1), the carbon source is sodium lignosulfonate, glucose or sucrose.
5. NaFeS as claimed in claim 12The preparation method of the/C composite material is characterized in that in the step (1), the ratio of Na to Fe to S to C =1: 1:2: 3.5-5.5 mol ratio.
6. NaFeS as claimed in claim 12The preparation method of the/C composite material is characterized in that in the step (1), the ratio of Na to Fe to S to C =1: 1:2: 4.2-4.6 mol ratio.
7. NaFeS as claimed in claim 12The preparation method of the/C composite material is characterized in that in the step (2), the grinding revolution number is 1200r min-1The grinding time is 100 min.
8. NaFeS as claimed in claim 12The preparation method of the/C composite material is characterized in that in the step (3), the temperature is heated to 300 ℃ and kept for 200min, and the temperature is continuously raised to 600 ℃ and kept for 480 min.
9. NaFeS as claimed in claim 12The preparation method of the/C composite material is characterized by comprising the following steps:
mixing 2.482g of sodium thiosulfate, 1.799g of ferrous oxalate and 0.685g of sucrose, adding absolute ethyl alcohol to submerge the solid powder, stirring, putting into a ball milling tank, and performing 1200r min-1Grinding for 100min at the rotating speed of (1) to obtain a paste mixture; drying the precursor at 60 ℃, and grinding the dried precursor into powder to obtain a precursor; finally heating the NaFeS to 300 ℃ in nitrogen atmosphere, preserving heat for 200min, then continuously heating to 600 ℃ and preserving heat for 480min, and naturally cooling to obtain NaFeS2a/C composite material.
10. The negative electrode material NaFeS of the novel sodium-ion battery prepared by the method of any one of claims 1 to 92Composite material/CAnd (5) feeding.
11. NaFeS prepared by the process of any one of claims 1-92The application of the/C composite material as the negative electrode material of the sodium-ion battery comprises the following steps:
firstly, NaFeS is put into2Fully grinding and uniformly mixing the conductive agent and the binder with the/C, adding an N-methyl pyrrolidone solvent, and uniformly stirring to obtain pre-coating slurry;
coating the precoating slurry on a copper foil, drying the electrode plate to obtain the negative electrode plate of the sodium-ion battery, and using the obtained negative electrode plate of the sodium-ion battery for the sodium-ion battery of the button type battery.
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Effective date of registration: 20210524 Address after: No.13, 3rd floor, building 1, No.1, Tidu street, Qingyang District, Chengdu, Sichuan 610031 Patentee after: Chengdu yishenrui Technology Co.,Ltd. Address before: 250353 University Road, Changqing District, Ji'nan, Shandong Province, No. 3501 Patentee before: Qilu University of Technology Effective date of registration: 20210524 Address after: 226600 No.162, Yong'an South Road, Hai'an hi tech Zone, Nantong City, Jiangsu Province Patentee after: JIANGSU CORE-CIRCLES AMPEREX TECHNOLOGY Co.,Ltd. Address before: No.13, 3rd floor, building 1, No.1, Tidu street, Qingyang District, Chengdu, Sichuan 610031 Patentee before: Chengdu yishenrui Technology Co.,Ltd. |
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