CN107195876B - A kind of preparation method and sodium-ion battery of Nanoscale Iron selenium sulfide - Google Patents
A kind of preparation method and sodium-ion battery of Nanoscale Iron selenium sulfide Download PDFInfo
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- CN107195876B CN107195876B CN201710288558.8A CN201710288558A CN107195876B CN 107195876 B CN107195876 B CN 107195876B CN 201710288558 A CN201710288558 A CN 201710288558A CN 107195876 B CN107195876 B CN 107195876B
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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
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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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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to transition metal selenium sulfide to prepare correlative technology field, it discloses a kind of preparation methods of Nanoscale Iron selenium sulfide, and the preparation method comprises the following steps: (1) purity is Prussian blue greater than 99% business, selenium powder of the purity greater than 99.9% and sulphur powder are sealed in the container full of inert atmosphere according to stoichiometric ratio；(2) by step (1)) in the container be sintered, be cooled to room temperature to obtain product；(3) product of acquisition is warming up under inert protective atmosphere 700 DEG C, and is kept for 4 hours, with the iron selenium sulfide for the nano-scale that the graphitization carbon-coating obtained by N doping coats.Sodium-ion battery the invention further relates to the iron selenium sulfide using preparation method as described above preparation as negative electrode material, product quality is high, raw material is easy to get, process is simple, equipment requirement is lower, and sodium-ion battery shows stable storage sodium performance, outstanding cyclical stability and good high rate performance.
Description
Technical field
The invention belongs to transition metal selenium sulfide to prepare correlative technology field, more particularly, to a kind of Nanoscale Iron selenium
The preparation method and sodium-ion battery of sulfide.
Background technique
Transition metal selenium sulphur compound is the general name for a kind of multicomponent material that metal and selenium sulphur are formed, and is had very important
Research significance and potential utility 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, iron selenium sulfide is expected in sodium-ion battery as negative
Pole material.
Fe2The synthetic method of SeS 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 ratio ingredient and raw material is fitted into high energy ball mill, after mixing by high-energy ball milling, will be produced
Object is fitted into corundum boat, and corundum boat is then put into tube furnace, under the conditions of inert atmosphere protection, as temperature gradient 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) open: 2015, Liu just used high temperature solid-state method to synthesize the crystal of iron selenium sulfide.
However, the phase that high temperature solid-state method generates is often impure, and the reaction time is longer；Meanwhile obtained particle shape
It is very uneven, and the granularity of particle is very big, all at 1 μm or more.In addition, at present to Fe2SeS nano particle cladding carbon-coating is ground
Study carefully less.Correspondingly, there is the technologies for developing a kind of method that can be simple and efficient synthesis Nanoscale Iron selenium sulfide for this field
Demand.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, the present invention provides a kind of preparations of Nanoscale Iron selenium sulfide
Method designs the preparation method of Nanoscale Iron selenium sulfide based on the preparation characteristic of existing iron selenium sulfide.It is described
The preparation method of nanometer iron wire sulfide passes through will be commercialized Prussian blue as source of iron, simple using process, low in cost
Preparation method Prussian blue, selenium powder and sulphur powder are reacted at a certain temperature directly generate by the graphitization carbon-coating of N doping
Nanoscale Iron selenium sulfide (such as Fe of cladding2SeS/C), it is severe thus to efficiently solve transition metal iron selenium sulfide synthesis condition
It carves, the problem that technique is cumbersome, product is impure, and the Nanoscale Iron selenium sulfide being prepared is by the graphitization carbon-coating packet of N doping
It covers 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, a kind of preparation side of Nanoscale Iron selenium sulfide is provided
Method comprising following steps:
(1) purity is Prussian blue greater than 99% business, selenium powder of the purity greater than 99.9% and sulphur powder are 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 under inert protective atmosphere 700 DEG C, and is 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 partial size of the iron selenium sulfide is 50nm~100nm；The graphitization carbon-coating of the N doping coats
The surface of the iron selenium sulfide is to form core-shell structure；The N doping graphitization carbon-coating with a thickness of 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 ratio between the selenium powder and the sulphur powder is 2:1.5:
1.5。
It is another aspect of this invention to provide that providing a kind of preparation method using Nanoscale Iron selenium sulfide as described above
Sodium-ion battery of the iron selenium sulfide of preparation as negative electrode material.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, it is provided by the invention to receive
The preparation method and sodium-ion battery of rice iron selenium sulfide mainly have the advantages that
(1) present invention is obtained by solid phase reaction by nitrogen using commercialized Prussian blue material as source of iron presoma
The Nanoscale Iron selenium sulfide that the graphitization carbon-coating of doping uniformly coats, product quality is high, raw material is easy to get, process is simple, equipment is wanted
Ask lower；
(2) present invention can be obtained nanometer of the grain diameter within the scope of 50nm~100nm by simple preparation method
Particle, while it being uniformly coated with the graphitization carbon-coating of N doping on the surface of particle, complete core-shell structure is formd, wherein
The thickness of carbon-coating is graphitized in 5nm~10nm, core-shell structure can not only prevent nanoparticle agglomerates, can also protect in nucleocapsid
Iron selenium sulfide；
(3) it can be applied in sodium-ion battery using iron selenium sulfide nanoparticle prepared by preparation method of the invention
As cathode, stable storage sodium performance, outstanding cyclical stability and good high rate performance are shown.
Detailed description of the invention
Fig. 1 is the flow diagram of the preparation method for the Nanoscale Iron selenium sulfide that embodiment of the present invention provides；
Fig. 2 is the iron selenium sulfide (Fe using the preparation method preparation of the Nanoscale Iron selenium sulfide in Fig. 12SeS/C)
XRD curve graph；
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 using the iron selenium sulfide (Fe in Fig. 22SeS/C) bent as the cyclic voltammetric of the sodium-ion battery of cathode
Line；
Fig. 6 is using the iron selenium sulfide (Fe in Fig. 22SeS/C) the charging and discharging curve as the sodium-ion battery of cathode；
Fig. 7 is using the iron selenium sulfide (Fe in Fig. 22SeS/C) the cycle performance figure as the sodium-ion battery of cathode.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
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 the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
Referring to Fig. 1, the preparation method for the Nanoscale Iron selenium sulfide that embodiment of the present invention provides mainly includes following step
It is rapid:
Step 1, purity is Prussian blue greater than 99% business, selenium powder of the purity greater than 99.9% and sulphur powder are according to change
Metering ratio is learned to be sealed in the container full of inert atmosphere.Specifically, the stoichiometric ratio is 2:1.5:1.5, wherein described
Commercially Prussian blue, the described selenium powder and the sulphur powder are to buy to obtain from market；The container is glass tube.
The container in step 1 is sintered, is cooled to room temperature to obtain product by step 2.Specifically, by institute
It states glass tube setting to be sintered in tube furnace, sintering temperature is 700 DEG C, and sintering time is 10 hours.
The product of acquisition is warming up under inert protective atmosphere 700 DEG C, and is kept for 4 hours by step 3, to obtain
The iron selenium sulfide of the nano-scale coated by the graphitization carbon-coating of N doping.Specifically, the partial size of the iron selenium sulfide
For 50nm~100nm.
It is appreciated that in other embodiments, stoichiometric ratio, burning between the Prussian blue, selenium powder of business and sulphur powder
The knot time and sintering temperature etc. is not limited to present embodiment, such as the Prussian blue stoichiometry between selenium powder and sulphur powder of business
Than being 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 prepared using the preparation method of Nanoscale Iron selenium sulfide provided by the invention is bent
Line chart, by being compared with XRD standard PDF card (shown in the lower part Fig. 2) it is found that using Nanoscale Iron provided by the invention
The iron selenium sulfide of the preparation method preparation of selenium sulfide is mutually pure phase.
Referring to Fig. 3, can be seen that from Fig. 3 using Nanoscale Iron selenium sulfide prepared by the present invention is mainly grain diameter
In the nano particle of 50~100nm.Referring to Fig. 4, can be seen that the grain diameter master of the Nanoscale Iron selenium sulfide from Fig. 4
Will be in 50~100nm, and the surface of the Nanoscale Iron selenium sulfide is uniformly coated and formd by the graphitization carbon-coating of N doping
Core-shell structure.
Fig. 5 to Fig. 7 is please 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 expression is vulcanized with Nanoscale Iron selenium
Object as negative electrode material sodium-ion battery from first lap to the cyclic voltammetry data of the 5th circle, the test be 0.01~
3.0V(vs Na+/ Na) section, using the scanning speed of 0.1mV/s, from test result as can be seen that the Nanoscale Iron selenium vulcanizes
Object shows stable storage sodium performance, and embedding sodium peak is shown near 1.39V, 1.21V and 0.65V, and 1.42V nearby shows to take off
Sodium peak；Charge and discharge density is 500mA/g in the experiment of 1 circle, the charging and discharging curve of 2 circles of the sodium-ion battery, 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 from the figure that negative electrode material of the Nanoscale Iron selenium sulfide as sodium-ion battery, that show beneficial to follow
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 of Nanoscale Iron selenium sulfide provided by the invention, use commercialized Prussia
Blue material is vulcanized as source of iron presoma by the Nanoscale Iron selenium that the graphitization carbon-coating that solid phase reaction obtains N doping uniformly coats
Object, product quality is high, raw material is easy to get, process is simple, equipment requirement is lower；It can be obtained particle by simple preparation method
Nano particle of the diameter within the scope of 50nm~100nm, while the graphitized carbon of N doping is uniformly coated on the surface of particle
Layer, forms complete core-shell structure, wherein the thickness of graphitization carbon-coating is in 5nm~10nm, core-shell structure can not only prevent from receiving
Rice grain is reunited, and the iron selenium sulfide in nucleocapsid can also be protected；The iron selenium sulfide prepared using preparation method of the invention
Nano particle can be applied in sodium-ion battery show stable storage sodium performance, outstanding stable circulation as cathode
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, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (6)
1. a kind of preparation method of Nanoscale Iron selenium sulfide, which is characterized in that method includes the following steps:
(1) purity is Prussian blue greater than 99% business, selenium powder of the purity greater than 99.9% and sulphur powder are according to stoichiometric ratio
It is sealed in the container full of inert atmosphere；
(2) container in step (1) is sintered, is cooled to room temperature to obtain product；Wherein, sintering temperature 650
DEG C~750 DEG C, sintering time is 10h~20h；
(3) product of acquisition is warming up under inert protective atmosphere 700 DEG C, and is kept for 4 hours, to obtain by N doping
Graphitization carbon-coating cladding nano-scale iron selenium sulfide, the graphitization carbon-coating of the N doping uniformly coats the iron selenium
The surface of sulfide is to form core-shell structure；Wherein, the partial size of the iron selenium sulfide is 50nm~100nm；The N doping
Graphitization carbon-coating with a thickness of 5nm~10nm.
2. the preparation method of Nanoscale Iron selenium sulfide as described in claim 1, it is characterised in that: the container is glass tube.
3. the preparation method of Nanoscale Iron selenium sulfide as described in claim 1, it is characterised in that: the container is in tube furnace
Inside it is sintered.
4. the preparation method of Nanoscale Iron selenium sulfide as described in claim 1, it is characterised in that: sintering temperature is 700 DEG C, is burnt
Tying the time is 10 hours.
5. the preparation method of Nanoscale Iron selenium sulfide as described in any one of claims 1-3, it is characterised in that: the business is general
Stoichiometric ratio between Shandong scholar indigo plant, the selenium powder and the sulphur powder is 2:1.5:1.5.
6. a kind of iron selenium sulfide prepared by the preparation method using the described in any item Nanoscale Iron selenium sulfide of claim 1-5
Sodium-ion battery as negative electrode material.
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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 |
| 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 |
| CN108539196B (en) * | 2018-05-15 | 2020-12-29 | 华中科技大学 | High-performance sulfur-based composite cathode 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 |
| 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 |
| CN112186182B (en) * | 2020-09-10 | 2021-05-18 | 青岛科技大学 | One-dimensional hollow carbon-coated iron selenide nanotube composite electrode material and preparation method 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 |
| CN112803017B (en) * | 2021-03-01 | 2022-09-13 | 吉林大学 | Hollow spherical bimetal chalcogenide, preparation method thereof and sodium battery cathode |
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| US7745047B2 (en) * | 2007-11-05 | 2010-06-29 | Nanotek Instruments, Inc. | Nano graphene platelet-base composite anode compositions for lithium ion batteries |
| CN102024938B (en) * | 2010-10-29 | 2013-04-24 | 北京工业大学 | C/Fe3C lithium ion battery negative material and preparation method thereof |
| CN102175728A (en) * | 2011-01-18 | 2011-09-07 | 兰州大学 | Method for preparing nanometer Co-Fe prussian-blue complex-carbon nano tube composite hydrogen peroxide sensor |
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