CN108172790A - A kind of nano-lithium fluoride/nickel ferrite based magnetic loaded cathode material compound and preparation method thereof - Google Patents
A kind of nano-lithium fluoride/nickel ferrite based magnetic loaded cathode material compound and preparation method thereof Download PDFInfo
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- CN108172790A CN108172790A CN201711421396.7A CN201711421396A CN108172790A CN 108172790 A CN108172790 A CN 108172790A CN 201711421396 A CN201711421396 A CN 201711421396A CN 108172790 A CN108172790 A CN 108172790A
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- lithium fluoride
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- ferrite based
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- nickel ferrite
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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 invention discloses a kind of nano-lithium fluoride/nickel ferrite based magnetic loaded cathode material compounds and preparation method thereof, and including lithium fluoride and nickel ferrite based magnetic loaded, the lithium fluoride and nickel ferrite based magnetic loaded molar ratio are 1:1‑1:5, the target used in pulsed laser deposition is made up of tabletting after lithium fluoride is mixed in proportion with the grinding of ferrous acid nickel material, the pulse laser wave that laser generates is incident to after lens focus on the target, and deposition obtains lithium fluoride nickel ferrite based magnetic loaded nano-complex film in argon gas atmosphere.The thickness of nano-complex membrane material of the present invention is 0.1 2 μm, lithium ion cell film electrode can be directly prepared into, electrode made of the film has good charging and discharging circulation reversibility, specific capacity is 200 300mAh/g for the first time, reversible specific capacity is 250mAh/g, and electrode capacity after 50 cycles still has 200mAh/g.And have the characteristics that chemical stability is good, specific capacity is high, preparation method is simple, suitable for lithium ion battery.
Description
Technical field
The invention belongs to technical field of lithium batteries in electrochemistry, are related to the cathode material for lithium ion battery, specially
A kind of nano-lithium fluoride/nickel ferrite based magnetic loaded cathode material compound and preparation method thereof.
Background technology
Lithium ion battery is the vital power supply of laptop, camera, mobile phone and other Communication Equipments, and have can
Automobile and other vehicles can be used for as green energy resource.Presently commercially available lithium ion battery mainly by carbon-based anode material,
Liquid organic electrolyte and transition metal oxide cathode material containing lithium are formed.In order to further improve lithium ion battery
Performance, people are studying, are finding new material more better than the electrode material performance used at present.In addition, with microelectronics
The miniaturization of device, the lithium ion battery that an urgent demand exploitation matches with this, such as film lithium ion battery etc..
Invention content
The present invention provides cathode material of lithium ion battery of good performance and preparation method thereof, this hair for the prior art
Bright the provided cathode material for lithium ion battery is a kind of lithium fluoride-nickel ferrite based magnetic loaded nano complexes material, such material
It, can be as the cathode material of high performance lithium ion battery with good chemical property.
The present invention is realized especially by following technical scheme：
A kind of nano-lithium fluoride/nickel ferrite based magnetic loaded cathode material compound, including lithium fluoride and nickel ferrite based magnetic loaded, passes through lithium fluoride and iron
Sour nickel material ground and mixed obtains lithium fluoride-nickel ferrite based magnetic loaded nano-complex thin-film material, the fluorine using pulsed laser deposition
It is 1 to change lithium and nickel ferrite based magnetic loaded molar ratio:1~1:5.
Preferably, the lithium fluoride and nickel ferrite based magnetic loaded molar ratio are 1:1.
Lithium fluoride-nickel ferrite based magnetic loaded nano-complex (LiF- of the present invention for cathode material for lithium ion battery
NiFe2O4) material is form of film, the thickness of thin-film material is 0.1-2 μm.
Lithium fluoride of the present invention-nickel ferrite based magnetic loaded nano-complex (LiF-NiFe2O4) material film can be directly prepared into lithium from
Sub- battery thin film electrode.
The present invention also provides the preparation method of the nano-lithium fluoride/nickel ferrite based magnetic loaded cathode material compound, especially by
Following steps are completed：Tabletting is made used in pulsed laser deposition after lithium fluoride is mixed in proportion with the grinding of ferrous acid nickel material
Target, the pulse laser wave that laser generates are incident to after lens focus on the target, and the distance of substrate and target is 40-60mm,
Deposition obtains lithium fluoride-nickel ferrite based magnetic loaded nano-complex (LiF-NiFe in argon gas atmosphere2O4) film.
Further, the substrate uses stainless steel substrates, platinized platinum or gold-plated monocrystalline silicon piece.
Further, the substrate temperature is 200-300 DEG C, it is preferred that the substrate temperature is 200 DEG C.
Further, the distance of the substrate and target is 50mm.
Further, the pulse laser wave that the laser generates is wavelength 248nm.
Further, the sedimentation time of film is required to determine by film thickness, generally 0.2-1 hours.Film thickness can be by
Scanning electron microscope measures, and the weight of film is obtained according to substrate weight difference before and after electronic balance weighing.
The crystal structure of lithium fluoride-nickel ferrite based magnetic loaded nano complexes material film is true by transmission electron microscope(TEM) in the present invention
It is fixed.
The nano-lithium fluoride/application of the ferrous acid nickel composite in lithium battery is prepared is also in protection scope of the present invention
It is interior.
Beneficial effects of the present invention：
In the present invention, by pulsed laser deposition, lithium fluoride-nickel ferrite based magnetic loaded nanometer obtained is answered on the substrates such as stainless steel substrates
Close object (LiF-NiFe2O4) material film electrode is respectively provided with charge-discharge performance, in voltage range 1.5-4.2V and current density 2uA/
cm2When, lithium fluoride-nickel ferrite based magnetic loaded nano-complex (LiF-NiFe2O4) material film electrode specific capacity 100 times cycle in protect
It holds in 150-200mAh/g.Therefore, lithium fluoride of the present invention-nickel ferrite based magnetic loaded nano-complex (LiF-NiFe2O4) it is a kind of novel the moon
Pole material has extensive prospect in applied to lithium ion battery.
Description of the drawings
Fig. 1 is lithium fluoride-nickel ferrite based magnetic loaded nano-complex (LiF-NiFe2O4) material film selective electron diffraction (SAED)
Image.
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, the technical solution in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other without making creative work
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
Lithium fluoride-ferrous acid of the present invention for cathode material for lithium ion battery is prepared using pulsed laser deposition
Nickel nano-complex (LiF-NiFe2O4) material film：By lithium fluoride and nickel oxide powder in molar ratio 1:Tabletting after 5 ground and mixeds
It is made the target used in pulsed laser deposition, the distance of stainless steel substrate and target is 50m, and substrate temperature is 200 DEG C, is produced by laser
Raw 248nm pulse lasers, laser beam are incident on after lens focus on target, frequency 10Hz, in argon gas atmosphere on substrate
Deposition 20 minutes, you can obtain lithium fluoride nickel ferrite based magnetic loaded nano-complex ((LiF-NiFe of the present invention2O4) film.
Transmission electron microscope(TEM) measures lithium fluoride made from above-described embodiment-nickel ferrite based magnetic loaded nano-complex (LiF-NiO) material
Material, the results are shown in Figure 1, lithium fluoride-nickel ferrite based magnetic loaded nanometer made from the bright method provided by the present invention of selective electron diffraction chart
Compound (LiF-NiO) material film.
To lithium fluoride nickel ferrite based magnetic loaded the nano-complex ((LiF-NiFe on stainless steel substrate2O4) membrane electrode electrochemistry
It can test, using the battery system being made of three electrodes, wherein, lithium fluoride-nickel ferrite based magnetic loaded nano-complex (LiF-NiFe2O4) material
Expect that film is used as working electrode, high-purity lithium piece is served as to electrode and reference electrode.Electrolyte is 1M LiPF6+EC+DMC
(V/V=1/1).Battery is assemblied in the charge-discharge test that battery is carried out in the drying box of applying argon gas in blue electric (Land) battery testing
It is carried out in system, it is as a result as follows：
Lithium fluoride-nickel ferrite based magnetic loaded nano-complex (LiF-NiFe2O4) membrane electrode can be in 2uA/cm2Under charge-discharge velocity into
Row charge and discharge cycles.In voltage range 1.5-4.2V, reversible capacity 200-300mAh/g, 50 capacity of cycle are maintained at
More than 200mAh/g.
Embodiment 2
Lithium fluoride-ferrous acid of the present invention for cathode material for lithium ion battery is prepared using pulsed laser deposition
Nickel nano-complex (LiF-NiFe2O4) material film：By lithium fluoride and nickel oxide powder in molar ratio 1:Tabletting after 2 ground and mixeds
It is made the target used in pulsed laser deposition, the distance of platinized platinum substrate and target is 40m, and substrate temperature is 300 DEG C, is generated by laser
248nm pulse lasers, laser beam are incident on after lens focus on target, frequency 10Hz, are sunk on substrate in argon gas atmosphere
Product 20 minutes, you can obtain lithium fluoride nickel ferrite based magnetic loaded nano-complex ((LiF-NiFe of the present invention2O4) film.
To lithium fluoride nickel ferrite based magnetic loaded the nano-complex ((LiF-NiFe on stainless steel substrate2O4) membrane electrode electrochemistry
It can test, using the battery system being made of three electrodes, wherein, lithium fluoride-nickel ferrite based magnetic loaded nano-complex (LiF-NiFe2O4) material
Expect that film is used as working electrode, high-purity lithium piece is served as to electrode and reference electrode.Electrolyte is 1M LiPF6+EC+DMC
(V/V=1/1).Battery is assemblied in the charge-discharge test that battery is carried out in the drying box of applying argon gas in blue electric (Land) battery testing
It is carried out in system, it is as a result as follows：
Lithium fluoride/nickel ferrite based magnetic loaded nano-complex (LiF-NiFe2O4) membrane electrode can be in 2uA/cm2Current density under into
Row charge and discharge cycles.In voltage range 1.5-4.2V, reversible capacity 180-220mAh/g, 50 capacity of cycle are maintained at
More than 190mAh/g.
Embodiment 3
Lithium fluoride-ferrous acid of the present invention for cathode material for lithium ion battery is prepared using pulsed laser deposition
Nickel nano-complex (LiF-NiFe2O4) material film：By lithium fluoride and nickel oxide powder in molar ratio 1:Tabletting after 1 ground and mixed
It is made the target used in pulsed laser deposition, the distance of gold-plated monocrystalline silicon piece substrate and target is 60m, and substrate temperature is 250 DEG C, by swashing
Light device generates 248nm pulse lasers, and laser beam is incident on after lens focus on target, frequency 10Hz, in argon gas atmosphere
Deposition on substrate 20 minutes, you can obtain lithium fluoride nickel ferrite based magnetic loaded nano-complex ((LiF-NiFe of the present invention2O4) film.
To lithium fluoride nickel ferrite based magnetic loaded the nano-complex ((LiF-NiFe on stainless steel substrate2O4) membrane electrode electrochemistry
It can test, using the battery system being made of three electrodes, wherein, lithium fluoride-nickel ferrite based magnetic loaded nano-complex (LiF-NiFe2O4) material
Expect that film is used as working electrode, high-purity lithium piece is served as to electrode and reference electrode.Electrolyte is 1M LiPF6+EC+DMC
(V/V=1/1).Battery is assemblied in the charge-discharge test that battery is carried out in the drying box of applying argon gas in blue electric (Land) battery testing
It is carried out in system, it is as a result as follows：
Lithium fluoride/nickel ferrite based magnetic loaded nano-complex (LiF-NiFe2O4) membrane electrode can be in 2uA/cm2Current density under into
Row charge and discharge cycles.In voltage range 1.5-4.2V, reversible capacity 200-250mAh/g, 50 capacity of cycle are maintained at
More than 180mAh/g.
4 comparative example of embodiment
Lithium fluoride and nickel ferrite based magnetic loaded in molar ratio 4:This electrode material can also be made in 1 ball milling 48 hours, and it is carried out
Electrochemical property test and above scheme have identical charging and discharging curve, but more than performance ratio poor.As a result it is as follows
Lithium fluoride/nickel ferrite based magnetic loaded nano-complex (LiF-NiFe2O4) electrode can be filled under the current density of 100mAh/g
Discharge cycles.In voltage range 1.5-4.2V, reversible capacity 150-200mAh/g, 50 capacity of cycle are maintained at
More than 140mAh/g.
In conclusion lithium fluoride of the present invention-nickel ferrite based magnetic loaded nano-complex (LiF-NiFe2O4) material film have it is good
Chemical property can be used as the cathode material of high performance lithium ion battery.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (9)
1. a kind of nano-lithium fluoride/nickel ferrite based magnetic loaded cathode material compound, which is characterized in that including lithium fluoride and nickel ferrite based magnetic loaded, pass through
Lithium fluoride and ferrous acid nickel material ground and mixed, lithium fluoride-nickel ferrite based magnetic loaded nano-complex film material is obtained using pulsed laser deposition
Material, the lithium fluoride and nickel ferrite based magnetic loaded molar ratio are 1:1~1:5.
2. a kind of nano-lithium fluoride/nickel ferrite based magnetic loaded cathode material compound according to described in claim 1, which is characterized in that described
Lithium fluoride and nickel ferrite based magnetic loaded molar ratio be 1:1.
3. a kind of nano-lithium fluoride/nickel ferrite based magnetic loaded cathode material compound according to described in claim 1, which is characterized in that described
Cathode material compound for form of film, the thickness of thin-film material is 0.1-2 μm.
4. the preparation method of nano-lithium fluoride described in claim 1/nickel ferrite based magnetic loaded cathode material compound, which is characterized in that logical
Cross following steps completion：Tabletting is made used in pulsed laser deposition after lithium fluoride is mixed in proportion with the grinding of ferrous acid nickel material
Target, the pulse laser wave that laser generates are incident to after lens focus on the target, and the distance of substrate and target is 40-60mm,
Deposition obtains lithium fluoride-nickel ferrite based magnetic loaded nano-complex film in argon gas atmosphere.
5. preparation method according to claim 4, which is characterized in that the substrate uses stainless steel substrates, platinized platinum or plating
Golden monocrystalline silicon piece.
6. preparation method according to claim 4, which is characterized in that the substrate temperature is 200-300 DEG C.
7. preparation method according to claim 4, which is characterized in that the substrate and the distance of target are 50mm.
8. preparation method according to claim 4, which is characterized in that the pulse laser wave that the laser generates is wave
Long 248nm.
9. nano-lithium fluoride described in claim 1/application of the ferrous acid nickel composite in lithium battery is prepared.
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| CN1735562A (en) * | 2003-01-17 | 2006-02-15 | 西巴特殊化学品控股有限公司 | A process for the production of porous inorganic materials or a matrix material containing nanoparticles |
| CN103094558A (en) * | 2012-12-18 | 2013-05-08 | 深圳市贝特瑞新能源材料股份有限公司 | Zinc-ferrite-based nanometer composite as well as preparation method and application thereof |
| CN105826550A (en) * | 2016-05-26 | 2016-08-03 | 广西师范大学 | Preparation method of lithium manganate cathode material with ferri-containing compound coating |
| CN105932247A (en) * | 2016-05-26 | 2016-09-07 | 广西师范大学 | Preparation method of nickel ferrite-coated lithium nickel manganese oxide positive electrode material |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1735562A (en) * | 2003-01-17 | 2006-02-15 | 西巴特殊化学品控股有限公司 | A process for the production of porous inorganic materials or a matrix material containing nanoparticles |
| CN103094558A (en) * | 2012-12-18 | 2013-05-08 | 深圳市贝特瑞新能源材料股份有限公司 | Zinc-ferrite-based nanometer composite as well as preparation method and application thereof |
| CN105826550A (en) * | 2016-05-26 | 2016-08-03 | 广西师范大学 | Preparation method of lithium manganate cathode material with ferri-containing compound coating |
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