CN107195876A - The preparation method and sodium-ion battery of a kind of Nanoscale Iron selenium sulfide - Google Patents
The preparation method and sodium-ion battery of a kind of Nanoscale Iron selenium sulfide Download PDFInfo
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- CN107195876A CN107195876A CN201710288558.8A CN201710288558A CN107195876A CN 107195876 A CN107195876 A CN 107195876A CN 201710288558 A CN201710288558 A CN 201710288558A CN 107195876 A CN107195876 A CN 107195876A
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- selenium sulfide
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- iron selenium
- nanoscale iron
- sodium
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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
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/36—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
- H01M4/581—Chalcogenides or intercalation compounds thereof
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
Correlative technology field is prepared the invention belongs to transition metal selenium sulfide, it discloses a kind of preparation method of Nanoscale Iron selenium sulfide, the preparation method comprises the following steps：(1) by purity be more than 99% business is Prussian blue, purity is more than 99.9% selenium powder and sulphur powder is sealed in the container full of inert atmosphere according to stoichiometric proportion；(2) by step (1)) in the container be sintered, be cooled to room temperature to obtain product；(3) product of acquisition is warming up to 700 DEG C under inert protective atmosphere, and kept for 4 hours, to obtain by the iron selenium sulfide of the nano-scale of the graphitization carbon-coating cladding of N doping.The invention further relates to sodium-ion battery of the iron selenium sulfide prepared using preparation method as described above as negative material, product quality is high, raw material is easy to get, process is simple, equipment requirement is relatively low, and sodium-ion battery shows stable storage sodium performance, outstanding cyclical stability and good high rate performance.
Description
Technical field
Correlative technology field is prepared the invention belongs to transition metal selenium sulfide, more particularly, to a kind of Nanoscale Iron selenium
The preparation method and sodium-ion battery of sulfide.
Background technology
Transition metal selenium sulphur compound is the general name of metal and a class multicomponent material of selenium sulphur formation, with very important
Research Significance and potential value.Iron selenium sulfide has the higher specific capacity of iron sulfide, while possessing iron selenides
Structural stability, and due to wherein containing electroactive iron, therefore iron selenium sulfide is expected in sodium-ion battery as negative
Pole material.
Fe2SeS synthetic method is concentrated mainly on high temperature solid-state method, and high temperature solid-state method is mainly with simple substance Fe, Se and S
For raw material, according to stoichiometric proportion dispensing and raw material is fitted into high energy ball mill, after being well mixed by high-energy ball milling, will produced
Thing is fitted into corundum boat, and corundum boat then is put into tube furnace, under the conditions of inert atmosphere protection, as thermograde is 700
DEG C keep 12 hours to be reacted, such as document (Jiabin Liu, Facile synthesis and electrochemical
properties of Fe2SeS for lithium ion batteries.J.Power.Sources.306(2016)317-
321) it is open：2015, Liu just synthesized the crystal of iron selenium sulfide using high temperature solid-state method.
However, the phase of high temperature solid-state method generation is often impure, and the reaction time is longer；Meanwhile, obtained particle profile
It is very uneven, and the granularity of particle is very big, all more than 1 μm.In addition, at present to Fe2SeS nano particles coat grinding for carbon-coating
Study carefully less.Correspondingly, this area, which is existed, develops a kind of technology for the method that can simply efficiently synthesize Nanoscale Iron selenium sulfide
Demand.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of preparation of Nanoscale Iron selenium sulfide
Method, its preparation characteristic based on existing iron selenium sulfide, the preparation method to Nanoscale Iron selenium sulfide is designed.It is described
The preparation method of nanometer iron wire sulfide is simple, with low cost using process by will be commercialized Prussian blue as source of iron
Preparation method cause Prussian blue, selenium powder and sulphur powder are reacted at a certain temperature to directly generate by the graphitization carbon-coating of N doping
Nanoscale Iron selenium sulfide (such as Fe of cladding2SeS/C), transition metal iron selenium sulfide synthesis condition is thus efficiently solved severe
Carve, the problem of technique is cumbersome, product is impure, and the Nanoscale Iron selenium sulfide prepared is by the graphitization carbon-coating bag of N doping
Cover uniformly, nanoparticle agglomerates can not only be prevented, iron selenium sulfide can also be protected.
To achieve the above object, according to one aspect of the present invention, there is provided a kind of preparation side of Nanoscale Iron selenium sulfide
Method, it comprises the following steps：
(1) by purity be more than 99% business is Prussian blue, purity is more than 99.9% selenium powder and sulphur powder is counted according to chemistry
Amount ratio is sealed in the container full of inert atmosphere；
(2) by step (1)) in the container be sintered, be cooled to room temperature to obtain product；
(3) product of acquisition is warming up to 700 DEG C under inert protective atmosphere, and kept for 4 hours, to obtain by nitrogen
The iron selenium sulfide of the nano-scale of the graphitization carbon-coating cladding of doping.
Further, the particle diameter of the iron selenium sulfide is 50nm~100nm；The graphitization carbon-coating cladding of the N doping
The surface of the iron selenium sulfide is to form core shell structure；The thickness of the graphitization carbon-coating of the N doping is 5nm~10nm.
Further, the container is glass tube.
Further, the container is sintered in tube furnace.
Further, sintering temperature is 650 DEG C~750 DEG C, and sintering time is 10h~20h.
Further, sintering temperature is 700 DEG C, and sintering time is 10 hours.
Further, the business is Prussian blue, the stoichiometric proportion between the selenium powder and the sulphur powder is 2:1.5:
1.5。
It is another aspect of this invention to provide that there is provided a kind of preparation method using Nanoscale Iron selenium sulfide as described above
The iron selenium sulfide of preparation as negative material sodium-ion battery.
In general, by the contemplated above technical scheme of the present invention compared with prior art, what the present invention was provided receives
The preparation method and sodium-ion battery of rice iron selenium sulfide mainly have the advantages that：
(1) present invention is obtained by nitrogen using commercialized Prussian blue material as source of iron presoma by solid phase reaction
The Nanoscale Iron selenium sulfide that the graphitization carbon-coating of doping is uniformly coated, product quality is high, raw material is easy to get, process is simple, equipment is wanted
Ask relatively low；
(2) present invention can obtain nanometer of the grain diameter in the range of 50nm~100nm by simple preparation method
Particle, while being uniformly coated with the graphitization carbon-coating of N doping on the surface of particle, forms complete core shell structure, wherein
The thickness of graphitization carbon-coating can not only prevent nanoparticle agglomerates in 5nm~10nm, core shell structure, can also protect in nucleocapsid
Iron selenium sulfide；
(3) the iron selenium sulfide nanoparticle prepared using the preparation method of the present invention can apply in sodium-ion battery
As negative pole, stable storage sodium performance, outstanding cyclical stability and good high rate performance is shown.
Brief description of the drawings
Fig. 1 is the schematic flow sheet of the preparation method for the Nanoscale Iron selenium sulfide that embodiment of the present invention is provided；
Fig. 2 is the iron selenium sulfide (Fe for using the preparation method of the Nanoscale Iron selenium sulfide in Fig. 1 to prepare2SeS/C)
XRD curve maps；
Fig. 3 is the iron selenium sulfide (Fe in Fig. 22SeS/C scanning electron microscope (SEM) photograph)；
Fig. 4 is the iron selenium sulfide (Fe in Fig. 22SeS/C perspective electron microscope)；
Fig. 5 is to use the iron selenium sulfide (Fe in Fig. 22SeS/C the cyclic voltammetric) as the sodium-ion battery of negative pole is bent
Line；
Fig. 6 is to use the iron selenium sulfide (Fe in Fig. 22SeS/C) as negative pole sodium-ion battery charging and discharging curve；
Fig. 7 is to use the iron selenium sulfide (Fe in Fig. 22SeS/C) as negative pole sodium-ion battery cycle performance figure.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below
Not constituting conflict each other can just be mutually combined.
Referring to Fig. 1, the preparation method for the Nanoscale Iron selenium sulfide that embodiment of the present invention is provided mainly includes following step
Suddenly：
Step one, by purity be more than 99% business is Prussian blue, purity be more than 99.9% selenium powder and sulphur powder according to change
Metering ratio is learned to be sealed in the container full of inert atmosphere.Specifically, the stoichiometric proportion is 2:1.5:1.5, wherein described
Commercially Prussian blue, described selenium powder and the sulphur powder are to buy to obtain from market；The container is glass tube.
Step 2, the container in step one is sintered, is cooled to room temperature to obtain product.Specifically, by institute
State glass tube and be arranged in tube furnace and be sintered, sintering temperature is 700 DEG C, sintering time is 10 hours.
Step 3,700 DEG C are warming up to by the product of acquisition under inert protective atmosphere, and are kept for 4 hours, to obtain
The iron selenium sulfide of the nano-scale coated by the graphitization carbon-coating of N doping.Specifically, the particle diameter of the iron selenium sulfide
For 50nm~100nm.
It is appreciated that in other embodiments, stoichiometric proportion, burning between the Prussian blue, selenium powder of business and sulphur powder
Knot time and sintering temperature etc. are not limited to present embodiment, such as the Prussian blue stoichiometry between selenium powder and sulphur powder of business
Than for 1~2, sintering temperature is 650 DEG C~750 DEG C, when sintering time is 10h~20h, can prepare the iron selenium of nano-scale
Sulfide.
Fig. 2 is that the XRD of the iron selenium sulfide of the preparation method preparation of the Nanoscale Iron selenium sulfide provided using the present invention is bent
Line chart, by being compared with XRD standard PDF cards (shown in Fig. 2 bottoms), the Nanoscale Iron provided using the present invention
Iron selenium sulfide prepared by the preparation method of selenium sulfide is mutually pure phase.
Referring to Fig. 3, can be seen that the Nanoscale Iron selenium sulfide mainly grain diameter prepared using the present invention from Fig. 3
In 50~100nm nano particle.Referring to Fig. 4, can be seen that the grain diameter master of the Nanoscale Iron selenium sulfide from Fig. 4
Will in 50~100nm, and the Nanoscale Iron selenium sulfide surface by the graphitization carbon-coating of N doping uniformly cladding and form
Core shell structure.
Fig. 5 to Fig. 7 is referred to, the Nanoscale Iron selenium prepared using the preparation method of Nanoscale Iron selenium sulfide of the present invention
Sulfide is assembled into sodium-ion battery as the cell negative electrode material of sodium ion, and wherein 1st to 5th expressions is vulcanized with Nanoscale Iron selenium
Thing as the sodium-ion battery of negative material from first lap to the cyclic voltammetry data of the 5th circle, the test be 0.01~
3.0V(vs Na+/ Na) it is interval, using 0.1mV/s sweep speed, from test result as can be seen that the Nanoscale Iron selenium vulcanizes
Thing shows stable storage sodium performance, shows to show to take off near embedding sodium peak, 1.42V near 1.39V, 1.21V and 0.65V
Sodium peak；The sodium-ion battery 1 circle, 2 circle charging and discharging curves experiment in discharge and recharge density be 500mA/g, can from figure
To find out, the discharge capacity of the Nanoscale Iron selenium sulfide has reached 387mAh/g, and charging capacity reaches 351mAh/g.In addition,
It can be seen that the Nanoscale Iron selenium sulfide is followed as the negative material of sodium-ion battery that show beneficial
Ring stability, after the circle of circulation 500, discharge capacity can also reach about 381mAh/g, and efficiency for charge-discharge has reached about
100%.
The preparation method and sodium-ion battery for the Nanoscale Iron selenium sulfide that the present invention is provided, it uses commercialized Prussia
Blue material is as source of iron presoma, the Nanoscale Iron selenium vulcanization that the graphitization carbon-coating for obtaining N doping by solid phase reaction is uniformly coated
Thing, product quality is high, raw material is easy to get, process is simple, equipment requirement is relatively low；Particle can be obtained by simple preparation method
Nano particle of the footpath in the range of 50nm~100nm, while being uniformly coated with the graphitized carbon of N doping on the surface of particle
Layer, forms complete core shell structure, the wherein thickness of graphitization carbon-coating is in 5nm~10nm, and core shell structure can not only prevent from receiving
Rice grain is reunited, and can also protect the iron selenium sulfide in nucleocapsid；The iron selenium sulfide prepared using the preparation method of the present invention
Nano particle can apply in sodium-ion battery as negative pole, show stable storage sodium performance, outstanding stable circulation
Property and good high rate performance.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, it is not used to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the invention etc., it all should include
Within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of Nanoscale Iron selenium sulfide, it is characterised in that this method comprises the following steps：
(1) by purity be more than 99% business is Prussian blue, purity be more than 99.9% selenium powder and sulphur powder according to stoichiometric proportion
It is sealed in the container full of inert atmosphere；
(2) by step (1)) in the container be sintered, be cooled to room temperature to obtain product；
(3) product of acquisition is warming up to 700 DEG C under inert protective atmosphere, and kept for 4 hours, to obtain by N doping
Graphitization carbon-coating cladding nano-scale iron selenium sulfide.
2. the preparation method of Nanoscale Iron selenium sulfide as claimed in claim 1, it is characterised in that：The grain of the iron selenium sulfide
Footpath is 50nm~100nm；The graphitization carbon-coating of the N doping coats the surface of the iron selenium sulfide to form core shell structure；
The thickness of the graphitization carbon-coating of the N doping is 5nm~10nm.
3. the preparation method of Nanoscale Iron selenium sulfide as claimed in claim 1, it is characterised in that：The container is glass tube.
4. the preparation method of Nanoscale Iron selenium sulfide as claimed in claim 1, it is characterised in that：The container is in tube furnace
Inside it is sintered.
5. the preparation method of the Nanoscale Iron selenium sulfide as described in claim any one of 1-4, it is characterised in that：Sintering temperature is
650 DEG C~750 DEG C, sintering time is 10h~20h.
6. the preparation method of Nanoscale Iron selenium sulfide as claimed in claim 5, it is characterised in that：Sintering temperature is 700 DEG C, is burnt
The knot time is 10 hours.
7. the preparation method of the Nanoscale Iron selenium sulfide as described in claim any one of 1-4, it is characterised in that：The business is general
Shandong scholar is blue, the stoichiometric proportion between the selenium powder and the sulphur powder is 2:1.5:1.5.
8. iron selenium sulfide prepared by a kind of preparation method of the Nanoscale Iron selenium sulfide described in use claim any one of 1-7
It is used as the sodium-ion battery of negative material.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108172406A (en) * | 2017-12-29 | 2018-06-15 | 山东大学 | One kind is with FeS2-xSexMaterial is the sodium ion capacitor of negative material |
| CN108394937A (en) * | 2018-03-26 | 2018-08-14 | 宁夏大学 | Vulcanize the preparation method of ferromanganese solid solution and its application as lithium ion battery negative material |
| CN108539196A (en) * | 2018-05-15 | 2018-09-14 | 华中科技大学 | A kind of high-performance sulfur-based composite anode material and preparation method thereof |
| CN110233264A (en) * | 2019-06-25 | 2019-09-13 | 复旦大学 | A kind of sodium-ion battery positive material and preparation method thereof of stratiform sulfoselenide as high rate capability |
| CN110280205A (en) * | 2019-06-26 | 2019-09-27 | 江西理工大学 | A kind of magnetism selenium doping iron-sulfur complex and its preparation method and application |
| CN111224098A (en) * | 2020-01-16 | 2020-06-02 | 南京信息工程大学 | Nitrogen-doped carbon modified FeSe negative electrode material for high-performance sodium battery and preparation method thereof |
| CN112186182A (en) * | 2020-09-10 | 2021-01-05 | 青岛科技大学 | One-dimensional hollow carbon-coated iron selenide nanotube composite electrode material and preparation method thereof |
| CN112803017A (en) * | 2021-03-01 | 2021-05-14 | 吉林大学 | Hollow spherical bimetal chalcogenide, preparation method thereof and sodium battery cathode |
| CN112960653A (en) * | 2021-01-29 | 2021-06-15 | 青岛科技大学 | Sulfur-doped iron selenide nanorod material and preparation method and application thereof |
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| CN108172406B (en) * | 2017-12-29 | 2020-04-21 | 山东大学 | FeS is used as a catalyst2-xSexSodium ion capacitor with negative electrode material |
| CN108172406A (en) * | 2017-12-29 | 2018-06-15 | 山东大学 | One kind is with FeS2-xSexMaterial is the sodium ion capacitor of negative material |
| CN108394937A (en) * | 2018-03-26 | 2018-08-14 | 宁夏大学 | Vulcanize the preparation method of ferromanganese solid solution and its application as lithium ion battery negative material |
| CN108394937B (en) * | 2018-03-26 | 2020-07-17 | 宁夏大学 | Preparation method of manganese iron sulfide solid solution and application of manganese iron sulfide solid solution as negative electrode material of lithium ion battery |
| CN108539196A (en) * | 2018-05-15 | 2018-09-14 | 华中科技大学 | A kind of high-performance sulfur-based composite anode material and preparation method thereof |
| CN110233264A (en) * | 2019-06-25 | 2019-09-13 | 复旦大学 | A kind of sodium-ion battery positive material and preparation method thereof of stratiform sulfoselenide as high rate capability |
| CN110280205B (en) * | 2019-06-26 | 2021-12-21 | 江西理工大学 | Magnetic selenium-doped iron-sulfur compound and preparation method and application thereof |
| CN110280205A (en) * | 2019-06-26 | 2019-09-27 | 江西理工大学 | A kind of magnetism selenium doping iron-sulfur complex and its preparation method and application |
| CN111224098A (en) * | 2020-01-16 | 2020-06-02 | 南京信息工程大学 | Nitrogen-doped carbon modified FeSe negative electrode material for high-performance sodium battery and preparation method thereof |
| CN112186182A (en) * | 2020-09-10 | 2021-01-05 | 青岛科技大学 | One-dimensional hollow carbon-coated iron selenide nanotube composite electrode material and preparation method thereof |
| CN112960653A (en) * | 2021-01-29 | 2021-06-15 | 青岛科技大学 | Sulfur-doped iron selenide nanorod material and preparation method and application thereof |
| CN112960653B (en) * | 2021-01-29 | 2022-07-22 | 青岛科技大学 | Sulfur-doped iron selenide nanorod material as well as preparation method and application thereof |
| CN112803017A (en) * | 2021-03-01 | 2021-05-14 | 吉林大学 | Hollow spherical bimetal chalcogenide, preparation method thereof and sodium battery cathode |
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