CN108461739A - A kind of high performance lithium ionic cell cathode material Fe7S8The preparation method of/C - Google Patents
A kind of high performance lithium ionic cell cathode material Fe7S8The preparation method of/C Download PDFInfo
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- CN108461739A CN108461739A CN201810247710.2A CN201810247710A CN108461739A CN 108461739 A CN108461739 A CN 108461739A CN 201810247710 A CN201810247710 A CN 201810247710A CN 108461739 A CN108461739 A CN 108461739A
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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
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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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/5815—Sulfides
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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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
The present invention relates to a kind of high performance lithium ionic cell cathode material Fe7S8The preparation method of/C, by source of iron Fe, sulphur source S, carbon source, surfactant is by ferro element：Element sulphur：Carbon source：Surfactant=1:(1.5~2.5):(1~2):The molar ratio of (0~0.5), which is mixed and added into solvent, stirs to obtain uniform mixed liquor；Mixed liquor is transferred in polytetrafluoroethyllining lining, heat reaction 10~48 hours, suction filtration or centrifuge washing after envelope kettle at 160~240 DEG C and dries to obtain black powder, as high performance lithium ionic cell cathode material Fe7S8/C.Raw material used herein is simple and easy to get, cheap, environmental-friendly, and time consumption and energy consumption is low, can high-volume low cost production；Single step reaction can synthesize in baking oven at a lower temperature, be not required to subsequent calcination, easy to operate, low for equipment requirements；Synthesis of organic substance iron-based presoma is needed in being reported before solving the problems, such as, while the pattern of product can to a certain extent be controlled by the way that surfactant is added again.
Description
Technical field
The present invention relates to a kind of high performance lithium ionic cell cathode material Fe7S8/ C belongs to electrochemistry and new energy materials skill
Art field.
Background technology
With the continuous social and economic development, demand of the people in terms of battery energy density is higher and higher.Lithium-ion electric
Pond has many advantages, such as that small, specific capacity is high, has extended cycle life as current most widely used energy storage device.But
Current commercialized lithium ion battery negative material is graphite, and specific capacity is relatively low, limits commercial batteries to a certain extent
Specific capacity brings some potential safety problems in addition, graphite cathode material will produce Li dendrite during charge and discharge cycles.Cause
This develops the lithium that novel specific capacity is higher, charge and discharge platform is relatively high to better meet the growing demand of people
Ion battery cathode material is a problem to be solved.
In recent years, transient metal sulfide becomes research heat because it has theoretical specific capacity more higher than commercial graphite
Point.In numerous transient metal sulfides, iron-based sulfide (such as FeS, FeS2And Fe3S4Deng) because it is with resourceful, valence
Lattice are cheap and advantages of environment protection and are widely studied and yield good result.In comparison, Fe7S8As novel
The report of negative material is relatively fewer, main reason is that Fe7S8Synthetic method it is complex and single.To improve Fe7S8's
Chemical property explores convenient, fast, simple synthetic method and realizes that the control of pattern is necessary simultaneously.
Related Fe at present7S8Research focus mostly in terms of magnetism, synthesis mostly use first synthesis presoma Fe (Ddtc)2
(Phen), method (Han W, the Gao M.Investigations on iron being then further pyrolyzed in oleyl amine
sulfide nanosheets prepared via a single-source precursor approach[J].Crystal
Growth and Design,2008,8(3):1023-1030.)(Zhang Y,Du Y,Xu H,et al.Diverse-
shaped iron sulfide nanostructures synthesized from a single source precursor
approach[J].CrystEngComm,2010,12(11):3658-3663.), mainly with FeSO4·7H2O, Phen water
Close object, sodium diethyldithiocarbamate trihydrate is raw material and needs to be reacted under nitrogen protection, entire reaction
Process is relatively complicated, condition is more harsh, and raw material is mostly organic matter, and certain pollution can be caused to environment.In addition, Fe7S8
Can by first synthesizing Fe-MOFs presomas or directly use iron powder, then through subsequently calcine to obtain with sulphur source (Huang W, Li S,
Cao X,et al.Metal–Organic Framework Derived Iron Sulfide–Carbon Core–Shell
Nanorods as a Conversion-Type Battery Material[J].ACS Sustainable Chemistry&
Engineering,2017,5(6):5039-5048.)(Kong X,Lou T,Li Y.Fe7S8nanorods and
nanosheets[J].Journal of alloys and compounds,2005,390(1-2):236-239.)(Li S,Qu
B,Huang H,et al.Controlled synthesis of iron sulfide coated by carbon layer
to improve lithium and sodium storage[J].Electrochimica Acta,2017,247:1080-
1087.).But subsequent calcination process is both needed to carry out under protection of argon gas, and need to strictly control reaction atmosphere, pressure and liter/
The problems such as rate of temperature fall, operation are relatively complicated.
In conclusion the Fe reported at present7S8The synthetic method of/C needs to synthesize by two-step method mostly, and synthesis material is more
Containing organic matter, process is cumbersome, energy consumption is more.
Invention content
In view of the deficiencies of the prior art, the present invention provides high-performance lithium ion electricity that is a kind of easy and being easy to industrialized production
Pond negative material Fe7S8The preparation method of/C, and there is preferable performance of lithium ion battery.
Technical scheme is as follows：
A kind of high performance lithium ionic cell cathode material Fe7S8The preparation method of/C, includes the following steps：
(1) source of iron Fe, sulphur source S, carbon source and surfactant are pressed into ferro element：Element sulphur：Carbon source：Surfactant=1:
(1.5~2.5):(1~2):The molar ratio of (0.1~0.5), which is mixed and added into solvent, stirs to obtain uniform mixed liquor；
(2) by mixed liquor made from step (1), 160~250 DEG C of heating are reacted 10~48 hours in confined conditions, are filtered
Or centrifuge washing and black powder is dried to obtain, as high performance lithium ionic cell cathode material Fe7S8/C。
According to currently preferred, the source of iron Fe described in step (1) is that ferric trichloride, ferric nitrate, ferric sulfate, sulfuric acid are sub-
Iron, iron ammonium sulfate, ferrous nitrate, one kind of frerrous chloride or arbitrary two or more combination；
It is further preferred that the source of iron Fe is ferric trichloride or ferric nitrate.
According to currently preferred, the sulphur source S described in step (1) is thiocarbamide, thioacetamide, solid-state sulfur powder, half
One kind in cystine or arbitrary two or more combination；Most preferably, the sulphur source S is thiocarbamide.
According to currently preferred, the carbon source described in step (1) is in ascorbic acid, glucose, fructose, maltose
A kind of or arbitrary two or more combination；It is further preferred that carbon source is ascorbic acid or glucose.
According to currently preferred, the surfactant described in step (1) is PVP (polyvinylpyrrolidone), SDS
(dodecyl sodium sulfate), SDBS (neopelex), one kind in CTAB (cetyl trimethylammonium bromide) or
Arbitrary two or more combination；Preferably, the surfactant is PVP.
According to currently preferred, the solvent described in step (1) is arbitrary two in deionized water, ethyl alcohol, ethylene glycol
Kind or two or more combinations；Further preferred solvent is the mixed solvent of deionized water and ethyl alcohol, most preferably deionized water
It is 1 with ethyl alcohol volume ratio:3 mixed solvent.
According to currently preferred, the addition volume of solvent and the molar ratio of ferro element are (1~4) in step (1)：1L/
Mol, i.e., one mole of source of iron, which is often added, will be added 1~4 liter of solvent.
According to currently preferred, heating reaction temperature is 180~240 DEG C in step (2), and the reaction time is 12~24 small
When.
The present invention uses solvent-thermal method, one-step synthesis Fe7S8/ C needs synthesis of organic substance iron-based in being reported before solving
The problem of presoma, raw material is simple and easy to get, and method is simple, while can be existed again to the pattern of product by the way that surfactant is added
It is controlled to a certain extent.
Advantages of the present invention is as follows：
(a) raw material used herein is simple and easy to get, cheap, environmental-friendly, can high-volume low cost production；
(b) reaction time of the invention is shorter, and time consumption and energy consumption is low, is conducive to practical application；
(c) the method for the present invention is simple, only needs single step reaction in baking oven at a lower temperature to generate final product, is wanted to equipment
Ask low；
(d) present invention not only may be implemented to provide carbon source by the way that the carbon source of reproducibility is added, can also be during the reaction
Realize Fe3+To Fe2+Reduction.
(e) products therefrom of the present invention generates in reaction process without poisonous and harmful substance without being post-processed.
(f) lithium ion battery negative material Fe produced by the present invention7S8/ C has excellent performance of lithium ion battery,
In 0.01~3.0V voltage ranges, when current density is 100mA/g, initial discharge capacity reaches 965.5mAh/g, is followed through 50 circles
It can reach 504.9mAh/g after ring.
Description of the drawings
Fig. 1 is product F e prepared by embodiment 17S8The XRD diffraction patterns of/C, wherein ordinate are intensity, and abscissa is diffraction
Angle (2 θ).
Fig. 2 is product F e prepared by embodiment 17S8The SEM photograph of/C.
Fig. 3 is the product F e that in test example 1 prepared by embodiment 17S8Cycle performances of/the C as lithium ion battery negative material
Figure, test electric current are 100mA/g；Wherein, ordinate is specific capacity, specific capacity unit：Every gram of milliampere hour (mAh/g), abscissa
It is the cycle number of turns (n).
Fig. 4 is the cycle performance figure for the product that in test example 2 prepared by comparative example 1, and test electric current is 100mA/g；Wherein, it indulges
Coordinate is specific capacity, specific capacity unit：Every gram of milliampere hour (mAh/g), abscissa are the cycle number of turns (n).
Specific implementation mode
Present invention will be further explained below with reference to specific examples.It should be understood that these examples are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after having read content set forth in the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed range.
Embodiment 1, Fe7S8The preparation of/C-material
By 10mmol FeCl3, 20mmol thiocarbamides, 15mmol ascorbic acid, 0.3g PVP are dissolved in 24mL mixed solvents
(water is 1 with ethyl alcohol volume ratio:3) it in, is transferred in polytetrafluoroethyllining lining after stirring evenly, envelope kettle is placed on 180 DEG C of baking ovens
Middle reaction 12 hours.After the completion of reaction final product is obtained by processes such as suction filtration, washing, drying.
Product is used Bruker D8ADVANCE x-ray powder diffraction instruments, and with Cu K alpha rays, (length scanning leg speed is
0.08 °/sec) material phase analysis is carried out, the results are shown in Figure 1, and as shown in Figure 1, final product is the Fe of pure phase7S8/ C, can be used as lithium
Ion battery negative electrode active material, Fig. 2 are the SEM photograph of final product, and photo shows that products therefrom is the micro- of nanometer sheet composition
Rice ball.
Embodiment 2, Fe7S8The preparation of/C-material
By 10mmol Fe (NO3)3, 25mmol thioacetamides, 15mmol glucose, 0.3g PVP be dissolved in 24mL mixing
(water is 1 with ethylene glycol volume ratio to solvent:3) it in, is transferred in polytetrafluoroethyllining lining after stirring evenly, envelope kettle is placed on 220
It is reacted 24 hours in DEG C baking oven.After the completion of reaction final product is obtained by processes such as suction filtration, washing, drying.
Product is used Bruker D8ADVANCE x-ray powder diffraction instruments, and with Cu K alpha rays, (length scanning leg speed is
0.08 °/sec) material phase analysis is carried out, as a result it is shown as the Fe of pure phase7S8/ C, can be used as lithium ion battery anode active material.
Embodiment 3, Fe7S8The preparation of/C-material
By 10mmol FeCl3, 20mmol cysteines, 20mmol ascorbic acid, be dissolved in 36mL mixed solvents (water with
Ethyl alcohol volume ratio is 1:1) it in, is transferred in polytetrafluoroethyllining lining after stirring evenly, envelope kettle, which is placed in 240 DEG C of baking ovens, to react
12 hours.After the completion of reaction final product is obtained by processes such as centrifugation, washing, drying.
Product is used Bruker D8ADVANCE x-ray powder diffraction instruments, and with Cu K alpha rays, (length scanning leg speed is
0.08 °/sec) material phase analysis is carried out, as a result it is shown as the Fe of pure phase7S8/ C, can be used as lithium ion battery anode active material.
Embodiment 4, Fe7S8The preparation of/C-material
By 10mmol FeSO4, 20mmol thiocarbamides, 15mmol glucose, 0.3g CTAB are dissolved in 30mL mixed solvent (water
It is 1 with ethylene glycol volume ratio:2) it in, is transferred in polytetrafluoroethyllining lining after stirring evenly, envelope kettle is placed in 200 DEG C of baking ovens
Reaction 12 hours.After the completion of reaction final product is obtained by processes such as suction filtration, washing, drying.
Product is used Bruker D8ADVANCE x-ray powder diffraction instruments, and with Cu K alpha rays, (length scanning leg speed is
0.08 °/sec) material phase analysis is carried out, as a result it is shown as the Fe of pure phase7S8/ C, can be used as lithium ion battery anode active material.
Comparative example 1
As described in Example 1, unlike：
Added-time, obtained product are not Fe to carbon source described in step (1)7S8, but its crystallinity is obviously deteriorated, and its pattern
Become blocky.
Comparative example 2
As described in Example 1, unlike：
Step (2) reaction time is 5 hours, cannot get Fe7S8。
Comparative example 3
As described in Example 1, unlike：
Step (2) reaction temperature is 120 DEG C, cannot get Fe7S8。
Comparative example 4
As described in Example 1, unlike：
Step (1) solvent is water, cannot get Fe7S8。
Test example 1, electrochemical property test
Final products prepared by embodiment 1 are used as lithium ion battery negative material, and electrode is prepared using rubbing method, will be former
Expect Fe in mass ratio7S8/C：Super P：CMC=70:20:10 ratio mixing, using water as solvent, is made negative electrode slurry, is coated in
On copper foil, slice obtains the pole piece of a diameter of 12mm after well-dried tabletting.Counter electrode of battery lithium piece.It is protected in inert gas
In the glove box of shield, with the LiPF of 1mol/L6For electrolyte, Celgerd 2300 is diaphragm, is assembled into 2320 type button cells.
Test equipment：Charge and discharge instrument (Land)；Fe is carried out on blue electric tester7S8/ C battery charging/discharging performance testings, knot
Fruit is as shown in Figure 3.
From the figure 3, it may be seen that charge and discharge electric condition：In 0.01~3.0V voltage ranges, when current density is 100mA/g, initially
Discharge capacity reaches 965.5mAh/g, can reach 504.9mAh/g after 50 circle cycles.
Test example 2
Product reference test example 1 made from comparative example 1 is tested into charge-discharge performance, the results are shown in Figure 4, comparison diagram 3,4
It is found that the charge-discharge performance of comparative example 1 is obviously deteriorated.
Claims (10)
1. a kind of high performance lithium ionic cell cathode material Fe7S8The preparation method of/C, includes the following steps：
(1) source of iron Fe, sulphur source S, carbon source and surfactant are pressed into ferro element：Element sulphur：Carbon source：Surfactant=1:(1.5
~2.5):(1~2):The molar ratio of (0.1~0.5), which is mixed and added into solvent, stirs to obtain uniform mixed liquor；
(2) by mixed liquor made from step (1) in confined conditions 160~250 DEG C heating reaction 10~48 hours, filter or from
The heart washs and dries to obtain black powder, as high performance lithium ionic cell cathode material Fe7S8/C。
2. high performance lithium ionic cell cathode material Fe according to claim 17S8The preparation method of/C, which is characterized in that
Source of iron Fe described in step (1) is ferric trichloride, ferric nitrate, ferric sulfate, ferrous sulfate, iron ammonium sulfate, ferrous nitrate, chlorine
Change ferrous one kind or arbitrary two or more combination.
3. high performance lithium ionic cell cathode material Fe according to claim 17S8The preparation method of/C, which is characterized in that
Sulphur source S described in step (1) be thiocarbamide, thioacetamide, solid-state sulfur powder, one kind in cysteine or it is arbitrary two kinds with
On combination.
4. high performance lithium ionic cell cathode material Fe according to claim 17S8The preparation method of/C, which is characterized in that
Carbon source described in step (1) is ascorbic acid, glucose, fructose, one kind in maltose or arbitrary two or more combination.
5. high performance lithium ionic cell cathode material Fe according to claim 17S8The preparation method of/C, which is characterized in that
Surfactant described in step (1) is one kind or arbitrary two or more combination in PVP, SDS, SDBS, CTAB.
6. high performance lithium ionic cell cathode material Fe according to claim 17S8The preparation method of/C, which is characterized in that
Solvent described in step (1) is two or more the arbitrary combination in deionized water, ethyl alcohol, ethylene glycol.
7. high performance lithium ionic cell cathode material Fe according to claim 67S8The preparation method of/C, which is characterized in that
Solvent described in step (1) is the mixed solvent of deionized water and ethyl alcohol.
8. high performance lithium ionic cell cathode material Fe according to claim 17S8The preparation method of/C, which is characterized in that
The addition volume of solvent and the molar ratio of ferro element are (1~4) in step (1)：1L/mol.
9. high performance lithium ionic cell cathode material Fe according to claim 17S8The preparation method of/C, which is characterized in that
Heating reaction temperature is 180~240 DEG C in step (2).
10. high performance lithium ionic cell cathode material Fe according to claim 17S8The preparation method of/C, feature exist
In the reaction time is 12~24 hours in step (2).
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| CN111162261A (en) * | 2020-01-14 | 2020-05-15 | 广东工业大学 | Iron disulfide/graphene oxide/nitrogen-doped multi-walled carbon nanotube composite material and preparation method and application thereof |
| CN111517374A (en) * | 2020-04-20 | 2020-08-11 | 鸡西市唯大新材料科技有限公司 | Fe7S8Preparation method of/C composite material |
| CN112209448A (en) * | 2020-08-27 | 2021-01-12 | 南京邮电大学 | Ultra-small FeS nanodot and preparation method and application thereof |
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| CN111517374B (en) * | 2020-04-20 | 2022-06-14 | 鸡西市唯大新材料科技有限公司 | Fe7S8Preparation method of/C composite material |
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Application publication date: 20180828 |