CN106898770A - The method that ferrite vulcanization prepares flower-shaped lithium cell cathode material iron sulphur compound - Google Patents
The method that ferrite vulcanization prepares flower-shaped lithium cell cathode material iron sulphur compound Download PDFInfo
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- CN106898770A CN106898770A CN201710194102.5A CN201710194102A CN106898770A CN 106898770 A CN106898770 A CN 106898770A CN 201710194102 A CN201710194102 A CN 201710194102A CN 106898770 A CN106898770 A CN 106898770A
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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
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- H01M4/5815—Sulfides
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- H—ELECTRICITY
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Abstract
The invention discloses the method that a kind of vulcanization of ferrite prepares flower-shaped lithium cell cathode material iron sulphur compound, using soluble ferric iron salt, glycol and diamines as raw material, there is micro-nano hollow ball structure ferrite by controlling reaction condition solvent heat to be obtained；Ferrite absolute ethyl alcohol is repeatedly washed, crystallinity ferrite hollow ball solid powder high is dried to obtain；Ferrite hollow ball solid powder is placed in tube furnace controls atmosphere ratio, heating rate and sintering temperature finally to prepare flower-shaped lithium cell cathode material iron sulphur compound.The present invention have the advantages that process is simple, it is easy to operate, be easy to regulate and control and it is with low cost, the characteristics of flower-shaped iron sulphur compound of gained is both easy to processing with micron ball, the characteristics of having nanometer sheet reactivity high again, and the excellent electrochemical performance of material, can be used as high-performance lithium cell negative electrode material, with preferable application prospect.
Description
Technical field
The invention belongs to the synthesis technical field of lithium cell cathode material, and in particular to a kind of ferrite vulcanization prepares flower-shaped
The method of lithium cell cathode material iron sulphur compound.
Background technology
Because lithium battery energy density is high, monomer voltage is high, good rate capability, small self discharge and the features such as environmental protection,
It is widely used in the fields such as digital product, electric motor car and electric automobile.Transient metal sulfide has excellent light, electricity, half
Conductor and magnetic property, are widely used in many fields.In recent years, transient metal sulfide attracts as new electrode material
Increasing sight, wherein transient metal sulfide pyrite（FeS2）It is high with its energy density（890mAh/g）, structure
Stablize, safety non-toxic is pollution-free and cheap, receives the attention of researcher, be a kind of lithium electricity of great application prospect
Pond negative material.But to there is self-conductance rate in iron sulphur compound relatively low, being formed in cyclic process many as negative material
Sulfide is easily soluble in electrolyte and volume increases the shortcomings of causing material structure heavy damage in charge and discharge process, causes
Stability and high rate performance in cyclic process is all poor, and them are hindered significantly in real-life application.Nano material
Because causing that it has special property, can solve by some special structure designs with special pattern and size
The problem that above-mentioned iron sulphur compound is faced as negative material.However, the method for the iron sulphur compound of synthesis is with very big at present
Limitation, such as synthesis temperature is too high, is difficult to keep original pattern；And the low knot for being difficult to take into account material of synthesis temperature
Brilliant degree, easily forms the material of undefined structure, and material property reduction is caused on the contrary.Therefore, current synthetic method is difficult to reality
The practical application of existing iron sulphur compound.
The content of the invention
Present invention solves the technical problem that there is provided a kind of ferrite vulcanization prepares flower-shaped lithium cell cathode material iron sulphur
The method of compound, property high is prepared using the ferrite hollow ball with special micro-nano structure under suitable vulcanization sintering temperature
Energy iron sulphur compound, can obtain crystallinity iron sulphur compound higher, and the micro-nano of its presoma ferrite can be fully kept again
Hollow ball structure, the micro-nano hollow ball structure has larger specific surface area, is conducive to storage lithium reaction, and micro-nano is hollow
Spherical structure is conducive to slowing down iron sulphur compound in charge and discharge process because of the negative effect that volumetric expansion brings, and then puies forward probe into Processing high Iron and Sulfur
The cycle performance of compound.
The present invention adopts the following technical scheme that ferrite vulcanization prepares flower-shaped cathode of lithium battery to solve above-mentioned technical problem
The method of material iron sulphur compound, it is characterised in that concretely comprise the following steps：
（1）Soluble ferric iron salt is dissolved in molysite mixed solution is obtained in mixed solution of the alcohol with amine, wherein soluble ferric iron salt is chlorine
Change one or more in iron, ferric sulfate, ferric nitrate or ferric acetate, alcohol and alcohol in the mixed solution of amine be ethylene glycol, propane diols,
One or more in butanediol, hexylene glycol, tripropylene glycol, triethylene glycol or pentanediol, alcohol is with amine in the mixed solution of amine
One or more in ethylenediamine, propane diamine, butanediamine, hexamethylene diamine, three propane diamine, triethylenediamine or pentanediamine；
（2）Molysite mixed solution is transferred to carry out solvent thermal reaction 6-36h and obtains with special in reactor in 100-300 DEG C
The ferrite mixture of micro-nano hollow ball structure；
（3）Ferrite mixture centrifugation is obtained with special micro-nano hollow ball structure after repeatedly being washed with organic solvent
Light green color ferrite, then be placed in baking oven dry, wherein organic solvent be absolute ethyl alcohol, acetone, hexamethylene, dimethyl sulfoxide or
One or more in tetrahydrofuran；
（4）Dried ferrite is placed in tube furnace, in the mixing of sulfurous gas atmosphere or inert gas and sulfurous gas
Under atmosphere, 300-600 DEG C of reaction 0.5-10h is warming up to the heating rate of 1-5 DEG C/min, is obtained with special after natural cooling
The flower-shaped lithium cell cathode material iron sulphur compound of high-performance of micro-nano hollow ball structure.
Further preferably, step（1）Described in molysite mixed solution in soluble ferric iron salt concentration for >=
0.001mmol/L。
The present invention has the advantages that compared with prior art：
1st, the micron ball that the obtained high-performance lithium cell negative electrode material iron sulphur compound of the present invention is made up of nanometer sheet, with spy
Different micro-nano hollow ball structure, micrometer structure is beneficial to the processing of later stage lithium cell cathode material, and nanometer sheet then ensure that material
Material has reactivity higher and can slow down because of the negative effect that volumetric expansion brings；
2nd, the present invention with the ferrite with micro-nano hollow ball structure be presoma, after the nanometer sheet of high activity can be substantially reduced
Phase prepares the sintering temperature of iron sulphur compound, can improve the crystallinity of material, the pattern of material can be kept again, and can have
Effect reducing energy consumption；
3rd, the features such as obtained iron sulphur compound of the present invention has discharge capacity high, good rate capability and has extended cycle life, is one
Plant high performance lithium cell cathode material；
4th, the present invention is prepared high-performance lithium cell negative electrode material iron sulphur compound by ferrite presoma, with equipment it is simple,
Easy to operate and with low cost the features such as, it is easy to commercial application.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph with micro-nano hollow ball structure ferrite；
Fig. 2 is the scanning electron microscope (SEM) photograph of iron sulphur compound obtained in the embodiment of the present invention 1；
Fig. 3 is the scanning electron microscope (SEM) photograph of iron sulphur compound obtained in the embodiment of the present invention 2；
Fig. 4 is the scanning electron microscope (SEM) photograph of iron sulphur compound obtained in the embodiment of the present invention 3；
Fig. 5 is the scanning electron microscope (SEM) photograph of iron sulphur compound obtained in the embodiment of the present invention 4；
Fig. 6 is the scanning electron microscope (SEM) photograph of iron sulphur compound obtained in the embodiment of the present invention 5.
Specific embodiment
The above of the invention is described in further details by the following examples, but this should not be interpreted as this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
By FeCl3•6H2O is dissolved in ethylene glycol and ethylenediamine, then mixed solution is transferred in reactor is carried out in 150 DEG C
Solvent thermal reaction 24h, cooling, centrifugation, absolute ethyl alcohol are washed 3 times, are dried, and ferrite intermediate are obtained, then by dry iron alcohol
Salt intermediate is placed in tube furnace, under argon gas and hydrogen sulfide gas mixed atmosphere, is warming up to the heating rate of 5 DEG C/min
300 DEG C of sintering 2h, natural cooling obtains iron sulphur compound, and Fig. 2 is the scanning electron microscope (SEM) photograph of iron sulphur compound obtained in the present embodiment.
Embodiment 2
By Fe2(SO4)3Be dissolved in propane diols and propane diamine, then mixed solution is transferred in reactor carried out in 150 DEG C it is molten
Agent thermal response 24h, cooling, centrifugation, absolute ethyl alcohol are washed 3 times, are dried, and ferrite intermediate are obtained, then by dry ferrite
Intermediate is placed in tube furnace, under argon gas and sulfur vapor mixed atmosphere, 450 DEG C of sintering is warming up to the intensification speed of 5 DEG C/min
2h, natural cooling obtains iron sulphur compound, and Fig. 3 is the scanning electron microscope (SEM) photograph of iron sulphur compound obtained in the present embodiment.
Embodiment 3
By Fe (NO)3Be dissolved in triethylene glycol and butanediamine, then mixed solution is transferred in reactor carried out in 150 DEG C it is molten
Agent thermal response 24h, cooling, centrifugation, absolute ethyl alcohol are washed 3 times, are dried, and ferrite intermediate are obtained, then by dry ferrite
Intermediate is placed in tube furnace, under argon gas and hydrogen sulfide gas mixed atmosphere, 600 is warming up to the heating rate of 1 DEG C/min
DEG C sintering 2h, natural cooling obtains iron sulphur compound, and Fig. 4 is the scanning electron microscope (SEM) photograph of iron sulphur compound obtained in the present embodiment.
Embodiment 4
By FeCl3•6H2O is dissolved in pentanediol and ethylenediamine, then mixed solution is transferred in reactor is carried out in 300 DEG C
Solvent thermal reaction 6h, cooling, centrifugation, tetrahydrofuran are washed 3 times, are dried, and ferrite intermediate are obtained, then by dry ferrite
Intermediate is placed in tube furnace, under ammonium sulfide vapor atmosphere, 450 DEG C of sintering 0.5h is warming up to the heating rate of 2 DEG C/min,
Natural cooling obtains iron sulphur compound, and Fig. 5 is the scanning electron microscope (SEM) photograph of iron sulphur compound obtained in the present embodiment.
Embodiment 5
By FeCl3•6H2O is dissolved in ethylene glycol and hexamethylene diamine, then mixed solution is transferred in reactor is carried out in 100 DEG C
Solvent thermal reaction 36h, cooling, centrifugation, acetone are washed 3 times, are dried, and ferrite intermediate are obtained, then by dry ferrite
Mesosome is placed in tube furnace, under nitrogen and hydrogen sulfide gas mixed atmosphere, 300 DEG C is warming up to the heating rate of 2 DEG C/min
Sintering 10h, natural cooling obtains iron sulphur compound, and Fig. 6 is the scanning electron microscope (SEM) photograph of iron sulphur compound obtained in the present embodiment.
Embodiment 6
Electrochemical property test：In mass ratio it is 8 by active material, conductive agent and adhesive:1:1 ratio mixing, adds N-
Methyl pyrrolidone is sized mixing and is made electrode slice, is dried and is weighed.The button electricity of CR2025 models is assembled into the glove box of argon gas
Pond, in blue electrical measurement test system after standing a night（Wuhan Jin Nuo electronics limited company, CT2001A）On carry out constant current density
Charge-discharge test, discharge current is 200mA/g, and electrochemical discharge the performance test results are shown in Table 1.
The electrochemical discharge the performance test results of table 1
| Synthesis condition | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Discharge capacity mAh/g first | 1500 | 1400 | 1200 | 1300 | 1400 |
| 100 circulation volume mAh/g | 890 | 890 | 780 | 800 | 850 |
It is of the invention to be advantageous in that：The ferrite of the special construction obtained by early stage solvent heat, can be in relatively low burning
Conversion reaction is carried out under junction temperature, and relatively low reaction temperature enables to its special appearance to be maintained, and then by control
Atmosphere, heating rate and sintering temperature during conversion reaction, further the structure of control products therefrom, composition and pattern, obtain
Obtain high performance lithium cell cathode material.Gained lithium cell cathode material specific capacity is high（200mA/g specific discharge capacities are
1400mAh/g）, platform voltage is low（0.5V）, cycle performance is excellent（100 circulation volume conservation rates are close to 70%）.Institute of the present invention
With method have the advantages that process is simple, it is easy to operate, be easy to regulation and control and it is with low cost, gained iron sulphur compound both have it is micro-
Rice ball be easy to processing the characteristics of, and with nanometer sheet reactivity it is high the characteristics of, and material excellent electrochemical performance, can use
Make high-performance lithium cell negative electrode material, with preferable application prospect.
Embodiment above describes general principle of the invention, principal character and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, simply original of the invention is illustrated described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements each fall within
In the scope of protection of the invention.
Claims (2)
1. the method that ferrite vulcanization prepares flower-shaped lithium cell cathode material iron sulphur compound, it is characterised in that concretely comprise the following steps：
（1）Soluble ferric iron salt is dissolved in molysite mixed solution is obtained in mixed solution of the alcohol with amine, wherein soluble ferric iron salt is chlorine
Change one or more in iron, ferric sulfate, ferric nitrate or ferric acetate, alcohol and alcohol in the mixed solution of amine be ethylene glycol, propane diols,
One or more in butanediol, hexylene glycol, tripropylene glycol, triethylene glycol or pentanediol, alcohol is with amine in the mixed solution of amine
One or more in ethylenediamine, propane diamine, butanediamine, hexamethylene diamine, three propane diamine, triethylenediamine or pentanediamine；
（2）Molysite mixed solution is transferred to carry out solvent thermal reaction 6-36h and obtains with special in reactor in 100-300 DEG C
The ferrite mixture of micro-nano hollow ball structure；
（3）Ferrite mixture centrifugation is obtained with special micro-nano hollow ball structure after repeatedly being washed with organic solvent
Light green color ferrite, then be placed in baking oven dry, wherein organic solvent be absolute ethyl alcohol, acetone, hexamethylene, dimethyl sulfoxide or
One or more in tetrahydrofuran；
（4）Dried ferrite is placed in tube furnace, in the mixing of sulfurous gas atmosphere or inert gas and sulfurous gas
Under atmosphere, 300-600 DEG C of reaction 0.5-10h is warming up to the heating rate of 1-5 DEG C/min, is obtained with special after natural cooling
The high performance lithium ionic cell cathode material iron sulphur compound of micro-nano hollow ball structure.
2. the method that ferrite vulcanization according to claim 1 prepares flower-shaped lithium cell cathode material iron sulphur compound, its
It is characterised by：Step（1）Described in molysite mixed solution in the concentration of soluble ferric iron salt be >=0.001mmol/L.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108878844A (en) * | 2018-06-30 | 2018-11-23 | 苏州思创源博电子科技有限公司 | A kind of preparation method of lithium battery iron sulphur negative electrode material |
| CN108899490A (en) * | 2018-06-19 | 2018-11-27 | 苏州思创源博电子科技有限公司 | A kind of preparation method of carbon-encapsulated iron sulphur composite negative pole material |
| CN111318259A (en) * | 2020-02-05 | 2020-06-23 | 江苏大学 | Iron alkoxide As5+Preparation method and application of ion remover |
| CN115231621A (en) * | 2022-08-26 | 2022-10-25 | 浙江理工大学 | Nano microspheric iron disulfide material and preparation method and application thereof |
| CN118380584A (en) * | 2024-06-24 | 2024-07-23 | 钛科(大连)新能源有限公司 | Lithium ion full battery with iron-sulfur compound cathode composition of more than 2V and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108899490A (en) * | 2018-06-19 | 2018-11-27 | 苏州思创源博电子科技有限公司 | A kind of preparation method of carbon-encapsulated iron sulphur composite negative pole material |
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| CN115231621A (en) * | 2022-08-26 | 2022-10-25 | 浙江理工大学 | Nano microspheric iron disulfide material and preparation method and application thereof |
| CN118380584A (en) * | 2024-06-24 | 2024-07-23 | 钛科(大连)新能源有限公司 | Lithium ion full battery with iron-sulfur compound cathode composition of more than 2V and preparation method thereof |
| CN118380584B (en) * | 2024-06-24 | 2024-08-30 | 钛科(大连)新能源有限公司 | Lithium ion full battery with iron-sulfur compound cathode composition of more than 2V and preparation method thereof |
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Application publication date: 20170627 |