CN106976847A - A kind of two selenizing ferrum nano materials and its synthetic method and application - Google Patents
A kind of two selenizing ferrum nano materials and its synthetic method and application Download PDFInfo
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- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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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
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- 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
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Abstract
The invention provides a kind of two selenizings ferrum nano material and its synthetic method and application, the nano material is flaky nanometer structure, additionally provides Hydrothermal Synthesiss FeSe2The synthetic method of nanometer sheet, using sodium borohydride reduction selenium powder, reacts with Iron trichloride hexahydrate, by controlling the consumption of Iron trichloride hexahydrate to prepare two selenizing iron materials again afterwards.This method controls to synthesize two selenizing iron materials of nano-scale under high pressure, compared with the conventional method, the present invention have preparation process is simple and quick, cost is low, environment amenable advantage, synthesized nano material has good electric conductivity, it is adaptable to electrochemical field.
Description
Technical field
The invention belongs to nano material synthesis and electrochemical field, specifically, be related to two selenizing ferrum nano materials and its
Synthetic method, its two ferrous selenide (FeSe synthesized2) have good electric conductivity, can as sodium-ion battery anode material.
Background technology
The problem of energy shortage and environmental pollution have become the very severe of today's society common concern, due to fossil combustion
Greenhouse effects are protruded the most caused by material burning, and this has had a strong impact on the life of people and health, thus find high-efficiency energy-storage and
Environment-friendly device turns into global focus.Due to high-energy-density and the advantage of environmental protection, lithium ion battery, sodium-ion battery etc. into
For up-and-coming candidate in energy storage device, smart mobile phone, notebook computer and electric automobile etc. have been widely applied to
Field.Compared with lithium ion battery, sodium aboundresources, consumption are low, and then sodium-ion battery causes the more interest of people.By
Higher than lithium ion radius and molal weight in sodium ion, sodium-ion battery capacity is low in charge and discharge process, short life, volume become
Change greatly, so suitable electrode material especially anode material serves key effect to the performance of sodium-ion battery.Therefore it is right
The research of sodium-ion battery anode material turns into a challenging problem.
Transition metal has good electric conductivity, transition metal oxide and sulfide as sodium-ion battery anode material
It has been be reported that, transition metal selenides and transition metal oxide, sulfide have a similar chemical property, but to this research compared with
It is few.Two ferrous selenide aboundresources, price are low, chemical property is stable, environment-friendly, nontoxic, are the suitable anodes of sodium-ion battery
Material.Zhang seminars (DOI:A kind of synthetic method of two ferrous selenides microballoon 10.1021/acsami.5b12148) is reported,
And it is have studied as the chemical property of sodium-ion battery anode material, but the microsphere diameter is larger (2-5 μm), is unfavorable for
Electrolyte is to material internal diffusion reaction.
Therefore, the target that the sodium-ion battery anode material with application value is always researchers is explored.
The content of the invention
The present invention provides a kind of two selenizings ferrum nano material and its synthetic method and application, and two selenizings are synthesized by hydro-thermal method
Iron nanometer sheet, the synthetic method craft is simple, easily operation, obtained two selenizings iron material as sodium-ion battery anode material
Material shows good chemical property.
The present invention is achieved using following technical scheme：
A kind of two selenizing ferrum nano materials, the nano material is flaky nanometer structure.
The present invention also provides a kind of ferrous selenide (FeSe of Hydrothermal Synthesiss two2) nanometer sheet synthetic method, specifically include following
Step：
1) deionized water of measured amounts is added in beaker, is passed through the oxygen in nitrogen removing water；
2) sodium borohydride and selenium powder are added to step 1) beaker in, magnetic agitation is allowed to react；
3) by the Iron trichloride hexahydrate (FeCl of certain mass3·6H2O) be added to step 1) beaker in, continue stir；
4) certain time is reacted, stops stirring, by step 1) liquid is transferred to autoclave in beaker, it is put into baking oven in certain
At a temperature of react.
5) after the completion of reacting, reactor cooling is taken out, product is washed, dried.
Step 1) in be passed through nitrogen except the oxygen in deionized water, required time is 20~50 minutes.
Step 2) sodium borohydride is as reducing agent, and the addition molar ratio range of its addition and selenium powder is 1~2:1 it
Between.
Step 3) Iron trichloride hexahydrate addition and selenium powder addition molar ratio range 0.5~1:Between 1.
Step 4) in liquid be transferred to after autoclave and can lead to nitrogen deoxygenation again, reaction temperature is 150~220 DEG C, during reaction
Between be 12~30h.
Application of the two selenizings ferrum nano material in terms of sodium-ion battery anode material.
The present invention is by the use of sodium borohydride as reducing agent, by simple Hydrothermal Synthesiss technology, under high pressure Fast back-projection algorithm
The selenizing Fe nanometer particles of sheet two.Because the electrochemical reaction of charge and discharge process only occurs in material surface, two-dimentional lamella knot
Structure exposure specific surface area is bigger, and bigger with electrolyte contacts area, avtive spot is more, and reaction is easier to occur, and capacity also has
Improved.Compared with prior art, the present invention has the advantages that preparation process is simple and quick, cost is low, environmentally friendly.
Two ferrous selenides prepare sodium-ion battery：
Obtained two selenizing iron materials are pressed 8 with acetylene black, sodium carboxymethylcellulose:1:1 ratio grinding, is ground to sense
By less than in the presence of having a particle, deionized water is added dropwise dropwise and continues grinding, it to a certain extent, is equably coated onto copper by grinding
On paper tinsel, first it is dried at room temperature, then be dried in vacuo 6h.It is a diameter of 12mm that the copper foil dried is cut into each with tablet press machine
Piece, then assembles sodium-ion battery in glove box, and battery size is CR2032 (3V).The battery assembled places more than 12h,
Constant current charge-discharge test can be carried out to it with blue electric tester, voltage range is 0.5V~2.9V, is surveyed with electrochemical workstation
Try cyclic voltammetry curve.
Compared with prior art, advantages and positive effects of the present invention are：It is simple, low that the present invention prepares nano material process
Consumption, it is easy to operate, obtained battery constant current charge-discharge is functional.
Brief description of the drawings
Fig. 1 is the scanning electron microscope diagram piece of two ferrous selenide nanometer sheets prepared by embodiment 1；
Fig. 2 is the transmission electron micrograph of two ferrous selenide nanometer sheets prepared by embodiment 1；
Fig. 3 is the high resolution transmission electron microscopy piece of two ferrous selenide nanometer sheets prepared by embodiment 1；
Fig. 4 is the XRD piece of two ferrous selenide nanometer sheets prepared by embodiment 1；
Fig. 5 is cycle performance picture of the sodium-ion battery of the preparation of embodiment 1 in the case where current density is 100mA/g；
Fig. 6 is high rate performance picture of the sodium-ion battery of the preparation of embodiment 1 under different current densities；
Fig. 7 is the sodium-ion battery of the preparation of embodiment 1 in the different cyclic voltammetry curve pictures swept under speed；
Fig. 8 is the picture of sodium-ion battery first three time of discharge and recharge under current density 100mA/g prepared by embodiment 1；
Fig. 9 is the scanning electron microscope diagram piece of two ferrous selenide nanometer sheets prepared by embodiment 2；
Figure 10 is the transmission electron micrograph of two ferrous selenide nanometer sheets prepared by embodiment 2；
Figure 11 is the scanning electron microscope diagram piece of two ferrous selenide nanometer sheets prepared by embodiment 3；
Figure 12 is the transmission electron micrograph of two ferrous selenide nanometer sheets prepared by embodiment 3；
Figure 13 is the transmission electron micrograph of two ferrous selenide nanometer sheets prepared by embodiment 4.
Embodiment
With reference to embodiment and accompanying drawing, the present invention will be further described in detail, but this explanation will not be constituted to this
The limitation of invention.
Embodiment 1
The preparation of the selenizing ferrum nano material of Hydrothermal Synthesiss two
Measure 40mL deionized waters to be added in beaker, be passed through the oxygen in nitrogen removing water.2mmol is added after 20min
Sodium borohydride and 1mmol selenium powder, carry out magnetic stir to solution become clarify.Then 0.5mmol Iron trichloride hexahydrate is added, after
Continuous stirring 10min, the process one leads directly to nitrogen.Stirring, which is finished, to be transferred to solution in reactor, continues logical nitrogen a little while, then
Lid is tightened, is put into baking oven, 24 hours are reacted at 180 DEG C.Reactor is taken out after completion of the reaction, dries in the air cool, in reactor
Product water and ethanol the difference centrifuge washing of precipitation several times, are finally dried in vacuo 12 hours at 60 DEG C.
Two selenizing iron materials derived above and acetylene black, sodium carboxymethylcellulose are pressed 8:1:1 ratio grinding, grinding
To being not felt by the presence of particle, deionized water is added dropwise dropwise and continues grinding, to a certain extent, it is equably applied for grinding
Onto copper foil, first it is dried at room temperature, then be dried in vacuo 6h.The copper foil dried is cut into each to be a diameter of with tablet press machine
12mm pieces, then assemble sodium-ion battery in glove box, and battery size is CR2032 (3V).The battery assembled places 12h
More than, constant current charge-discharge test can be carried out to it with blue electric tester, voltage range is 0.5V~2.9V, uses electrochemical operation
Test loop of standing volt-ampere curve.
Fig. 1 is the scanning electron microscope diagram piece of two ferrous selenide nanometer sheets prepared by embodiment 1, it can be seen that the two of synthesis
Selenizing ferrum nano material is laminated structure.
Fig. 2 is the transmission electron micrograph of two ferrous selenide nanometer sheets prepared by embodiment 1, it can be seen that the two of synthesis
Selenizing ferrum nano material is that laminated structure is consistent with scanning electron microscope diagram piece.
Fig. 3 is the high resolution transmission electron microscopy piece of two ferrous selenide nanometer sheets prepared by embodiment 1, it can be seen that closed
Into two selenizing ferrum nano material (1,1,1) crystal face interlamellar spacings be 0.257nm.
Fig. 4 is the XRD piece of two ferrous selenide nanometer sheets prepared by embodiment 1, it can be seen that the two ferrous selenides nanometer of synthesis
Material diffraction peak intensity is very strong, so two selenizing ferrum nano material crystallinity of synthesis are fine.
Fig. 5 is cycle performance picture of the sodium-ion battery in the case where current density is 100mA/g prepared by embodiment 1, can be with
Find out that the circle of battery discharge 50 specific capacity is 438.7mAh g under low current density-1, cycle performance is sufficiently stable, and coulombic efficiency connects
Nearly 100%.
Fig. 6 is high rate performance picture of the sodium-ion battery of the preparation of embodiment 1 under different current densities, in different electric currents
The circle specific capacity quite stable of discharge and recharge 5 is distinguished under density, and is 0.1Ag in current density-1、0.2Ag-1、0.4Ag-1、0.8Ag-1、
1.0Ag-1、2.0Ag-1Under specific discharge capacity be respectively 496mAh g-1、449mAh g-1、415mAh g-1、375mA h g-1、
360mAh g-1、307mAh g-1。
Fig. 7 is that the sodium-ion battery difference of the preparation of embodiment 1 sweeps the cyclic voltammetry curve picture under speed, and sweeping speed is respectively
0.2mV/s, 0.4mV/s, 0.6mV/s, 0.8mV/s, 1.0mV/s, it can be seen that have an oxidation peak and three reduction peaks.
Fig. 8 be embodiment 1 prepare sodium-ion battery under current density 100mA/g first three loop graph piece of discharge and recharge.
Embodiment 2
The preparation of the selenizing ferrum nano material of Hydrothermal Synthesiss two
Measure 40mL deionized waters to be added in beaker, be passed through the oxygen in nitrogen removing water.2mmol is added after 20min
Sodium borohydride and 1mmol selenium powder, carry out magnetic stir to solution become clarify.Then 0.6mmol Iron trichloride hexahydrate is added, after
Continuous stirring 10min, the process one leads directly to nitrogen.Stirring, which is finished, to be transferred to solution in reactor, continues logical nitrogen a little while, then
Lid is tightened, is put into baking oven, 24 hours are reacted at 180 DEG C.Reactor is taken out after completion of the reaction, dries in the air cool, in reactor
Product water and ethanol the difference centrifuge washing of precipitation several times, are finally dried in vacuo 12 hours at 60 DEG C.
Assembled battery part be the same as Example 1.
Fig. 9 is the scanning electron microscope diagram piece of two ferrous selenide nanometer sheets prepared by embodiment 2.
Figure 10 is the transmission electron micrograph of two ferrous selenide nanometer sheets prepared by embodiment 2, it can be seen that synthesis
Two ferrous selenide nanometer sheets are stacked.
Embodiment 3
The preparation of the selenizing ferrum nano material of Hydrothermal Synthesiss two
Measure 40mL deionized waters to be added in beaker, be passed through the oxygen in nitrogen removing water.2mmol is added after 20min
Sodium borohydride and 1mmol selenium powder, carry out magnetic stir to solution become clarify.Then 1.0mmol Iron trichloride hexahydrate is added, after
Continuous stirring 10min, the process one leads directly to nitrogen.Stirring, which is finished, to be transferred to solution in reactor, continues logical nitrogen a little while, then
Lid is tightened, is put into baking oven, 24 hours are reacted at 180 DEG C.Reactor is taken out after completion of the reaction, dries in the air cool, in reactor
Product water and ethanol the difference centrifuge washing of precipitation several times, are finally dried in vacuo 12 hours at 60 DEG C.
Assembled battery part be the same as Example 1.
Figure 11 is the scanning electron microscope diagram piece of two ferrous selenide nanometer sheets prepared by embodiment 3.
Figure 12 is the transmission electron micrograph of two ferrous selenide nanometer sheets prepared by embodiment 3, it can be seen that synthesis
Two ferrous selenide nanometer sheets are into coherent condition.
Embodiment 4
The preparation of the selenizing ferrum nano material of Hydrothermal Synthesiss two
Measure 40mL deionized waters to be added in beaker, be passed through the oxygen in nitrogen removing water.2mmol is added after 20min
Sodium borohydride and 1mmol selenium powder, carry out magnetic stir to solution become clarify.Then 0.5mmol nine water ferric nitrates are added, after
Continuous stirring 10min, the process one leads directly to nitrogen.Stirring, which is finished, to be transferred to solution in reactor, continues logical nitrogen a little while, then
Lid is tightened, is put into baking oven, 24 hours are reacted at 180 DEG C.Reactor is taken out after completion of the reaction, dries in the air cool, in reactor
Product water and ethanol the difference centrifuge washing of precipitation several times, are finally dried in vacuo 12 hours at 60 DEG C.
Assembled battery part be the same as Example 1.
Figure 13 is the transmission electron micrograph of two ferrous selenide nanometer sheets prepared by embodiment 4.
The above described is only a preferred embodiment of the present invention, being not the limitation for making other forms to the present invention, appoint
What those skilled in the art can be changed or be modified as the equivalent of equivalent variations using the technology contents of the disclosure above
Embodiment.But it is every without departing from technical solution of the present invention content, the technical spirit according to the present invention is made to above example
Any simple modification, equivalent variations and remodeling, still fall within the protection domain of technical solution of the present invention.
Claims (8)
1. a kind of two selenizings ferrum nano material, it is characterised in that：The nano material is flaky nanometer structure.
2. a kind of synthetic method of the ferrous selenide nanometer sheet of Hydrothermal Synthesiss two, it is characterised in that comprise the following steps：
1) deionized water of measured amounts is added in beaker, is passed through the oxygen in nitrogen removing water；
2) sodium borohydride and selenium powder are added to step 1) beaker in, magnetic agitation is allowed to react；
3) by the Iron trichloride hexahydrate (FeCl of certain mass3·6H2O) be added to step 1) beaker in, continue stir；
4) certain time is reacted, stops stirring, by step 1) liquid is transferred to autoclave in beaker, it is put into baking oven in certain temperature
Lower reaction；
5) after the completion of reacting, reactor cooling is taken out, product is washed, dried.
3. synthetic method according to claim 2, it is characterised in that：Step 1) in be passed through nitrogen except the oxygen in deionized water
Gas, required time is 20~50 minutes.
4. synthetic method according to claim 2, it is characterised in that：Step 2) in sodium borohydride as reducing agent, it adds
Enter the addition molar ratio range of amount and selenium powder 1~2:Between 1.
5. synthetic method according to claim 2, it is characterised in that：Step 3) in Iron trichloride hexahydrate addition and selenium powder
Addition molar ratio range 0.5~1:Between 1.
6. synthetic method according to claim 2, it is characterised in that：Step 4) in liquid be transferred to after autoclave and can lead to again
Nitrogen deoxygenation.
7. synthetic method according to claim 2, it is characterised in that：Step 4) in reaction temperature be 150~220 DEG C, instead
It is 12~30h between seasonable.
8. the answering in terms of sodium-ion battery anode material of two selenizing ferrum nano materials any one of the claims 1-7
With.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108977827A (en) * | 2018-08-01 | 2018-12-11 | 兰州大学 | Include FeSe2-Co3O4Composite material and preparation method and catalyst and application |
| 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 |
| CN113991185A (en) * | 2021-10-29 | 2022-01-28 | 世一国际新能源有限公司 | Energy storage lithium ion battery based on nano electrode and preparation method thereof |
| CN113991062A (en) * | 2021-10-29 | 2022-01-28 | 世一国际新能源有限公司 | High-capacity energy storage lithium ion battery and preparation method thereof |
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| CN101012054A (en) * | 2007-01-04 | 2007-08-08 | 山东师范大学 | Method of synthesizing cadmium selenide nano stick and use thereof |
| CN104477857A (en) * | 2014-12-03 | 2015-04-01 | 上海交通大学 | Two-dimensional ultrathin ferric diselenide nano material as well as preparation method and application thereof |
| CN105060261A (en) * | 2015-09-23 | 2015-11-18 | 广东工业大学 | Method for preparing ferrum diselenide self-assembled microflowers |
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| CN101012054A (en) * | 2007-01-04 | 2007-08-08 | 山东师范大学 | Method of synthesizing cadmium selenide nano stick and use thereof |
| CN104477857A (en) * | 2014-12-03 | 2015-04-01 | 上海交通大学 | Two-dimensional ultrathin ferric diselenide nano material as well as preparation method and application thereof |
| CN105060261A (en) * | 2015-09-23 | 2015-11-18 | 广东工业大学 | Method for preparing ferrum diselenide self-assembled microflowers |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108977827A (en) * | 2018-08-01 | 2018-12-11 | 兰州大学 | Include FeSe2-Co3O4Composite material and preparation method and catalyst and application |
| CN108977827B (en) * | 2018-08-01 | 2020-08-28 | 兰州大学 | Comprising FeSe2-Co3O4Composite material and preparation method thereof, catalyst and application |
| 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 |
| CN113991185A (en) * | 2021-10-29 | 2022-01-28 | 世一国际新能源有限公司 | Energy storage lithium ion battery based on nano electrode and preparation method thereof |
| CN113991062A (en) * | 2021-10-29 | 2022-01-28 | 世一国际新能源有限公司 | High-capacity energy storage lithium ion battery and preparation method thereof |
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