CN108400318A - Preparation method of cobaltosic oxide-ferric oxide composite oxide - Google Patents
Preparation method of cobaltosic oxide-ferric oxide composite oxide Download PDFInfo
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- CN108400318A CN108400318A CN201810039328.2A CN201810039328A CN108400318A CN 108400318 A CN108400318 A CN 108400318A CN 201810039328 A CN201810039328 A CN 201810039328A CN 108400318 A CN108400318 A CN 108400318A
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- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title abstract 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 44
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 24
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000001354 calcination Methods 0.000 claims abstract description 22
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 22
- 239000010941 cobalt Substances 0.000 claims abstract description 22
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000013256 coordination polymer Substances 0.000 claims abstract description 22
- 229920001795 coordination polymer Polymers 0.000 claims abstract description 22
- 229910052742 iron Inorganic materials 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 19
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 16
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 claims description 20
- 238000004321 preservation Methods 0.000 claims description 19
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
- 150000002506 iron compounds Chemical class 0.000 description 5
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012621 metal-organic framework Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 229910018095 Ni-MH Inorganic materials 0.000 description 1
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- 229910018477 Ni—MH Inorganic materials 0.000 description 1
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- 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
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a preparation method of cobaltosic oxide-ferric oxide composite oxide, which comprises the following steps: s1, co-dissolving cobalt dichloride, ferric nitrate, 1,3, 5-benzenetricarboxylic acid and hydrofluoric acid in water, stirring, heating, and preserving heat to obtain a cobalt/iron coordination polymer; and S2, calcining the cobalt/iron coordination polymer, and cooling to obtain the cobaltosic oxide-ferric oxide composite oxide. According to the invention, a simple and effective hydrothermal method is adopted to synthesize the cobalt/iron coordination polymer, and then the cobalt/iron coordination polymer is pyrolyzed, so that the obtained cobaltosic oxide-ferric oxide composite oxide has small and uniform particle size and excellent cycle performance.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of cobaltosic oxide-di-iron trioxide composite oxygen
The preparation method of compound.
Background technology
In contemporary society, the problems such as energy crisis and global warming, becomes increasingly severe, develops clean, reproducible new
The energy becomes to be even more important and crucial.Lithium rechargeable battery has height relative to lead-acid accumulator, Ni-MH battery, Ni-Cr battery
Operating voltage, high ratio energy the advantages that, therefore have been widely used.
Metal-organic framework materials have many advantages, such as adjustable more skies, structure and function, have been applied to perhaps
Mostly new field, such as new Chemical Decomposition, sensor, catalysis reaction and energy stores etc..Graphite electrode material due to compared with
The shortcomings of low theoretical specific capacity and density, it cannot meet people and lithium ion battery high-energy density and portability have been wanted
It asks, exploitation excellent electrochemical performance new material is current lithium ion battery urgent problem.Transition metal oxide is one
The conversion hysteria cathode of quasi-representative, but transition metal oxide (such as cobaltosic oxide, di-iron trioxide) exists and for the first time can not
The shortcomings of inverse capacitance loss is big, cycle life difference and poor high rate performance, in recent years, metal organic framework compound (MOFs) is
Through being obtained the nano material of homogeneous structural by calcining as unique presoma.
Invention content
Technical problems based on background technology, it is compound that the present invention proposes a kind of cobaltosic oxide-di-iron trioxide
The preparation method of oxide, the present invention synthesize cobalt/iron coordination polymer using simple and effective hydro-thermal method first, then to cobalt/iron
Coordination polymer is pyrolyzed, and obtained cobaltosic oxide-di-iron trioxide composite oxide particle is small and size uniformity, has
Excellent cycle performance.
A kind of preparation method of cobaltosic oxide-di-iron trioxide composite oxides proposed by the present invention, including walk as follows
Suddenly：
S1, by cobaltous dichloride, ferric nitrate, 1,3,5- benzenetricarboxylic acids, hydrofluoric acid are codissolved in water, are put into magnetic stir bar,
Stir at room temperature, take out stirrer, be put into polytetrafluoroethyllining lining, be subsequently placed into reaction kettle, heat up, heat preservation, obtain cobalt/
Iron coordination polymer；
S2, cobalt/iron coordination polymer is calcined in tube furnace ,-three oxygen of cobaltosic oxide is obtained after natural cooling
Change two iron compound oxides.
Preferably, in S1, the time of stirring is 0.5-3h.
Preferably, in S1, the temperature of heat preservation is 160-170 DEG C.
Preferably, in S1, the time of heat preservation is 72-80h.
Preferably, in S2, calcining carries out in the atmosphere of air.
Preferably, in S2, during calcining, the rate of heating is 1-5 DEG C/min.
Preferably, in S2, the temperature of calcining is 400-600 DEG C.
Preferably, in S2, the time of calcining is 1-4h.
Preferably, the cobaltous dichloride, ferric nitrate, 1,3,5- benzenetricarboxylic acids, hydrofluoric acid molar ratio be 2.3-2.5：2-
6：2-5：1-4.
Preferably, the molal volume (mmol/ml) of the cobaltous dichloride and water is than being 2.3-2.5：35-40.
The present invention synthesizes cobalt/iron coordination polymer using simple and effective hydro-thermal method first, then to cobalt/iron coordination polymer
It is pyrolyzed, obtained cobaltosic oxide-di-iron trioxide composite oxide particle is small and size uniformity, has excellent cycle
Performance, and its unique " worm " shape nanostructure, cushioning effect is played during removal lithium embedded to the volume expansion of material.
Description of the drawings
Fig. 1 is the SEM testing result schematic diagrames for cobaltosic oxide-di-iron trioxide composite oxides that the present invention obtains.
Fig. 2 is that the X-ray diffraction testing result for cobaltosic oxide-di-iron trioxide composite oxides that the present invention obtains is shown
It is intended to.
Fig. 3 is the cycle life and high rate performance test result schematic diagram of lithium ion button shape cell in test example 1 of the present invention.
Specific implementation mode
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of cobaltosic oxide-di-iron trioxide composite oxides, includes the following steps：
S1, by cobaltous dichloride, ferric nitrate, 1,3,5- benzenetricarboxylic acids, hydrofluoric acid are codissolved in water, stirring, be put into polytetrafluoro
It in ethylene liner, is subsequently placed into reaction kettle, heats up, heat preservation obtains cobalt/iron coordination polymer；
S2, cobalt/iron coordination polymer is calcined, cobaltosic oxide-di-iron trioxide combined oxidation is obtained after cooling
Object.
Embodiment 2
A kind of preparation method of cobaltosic oxide-di-iron trioxide composite oxides, includes the following steps：
S1, by cobaltous dichloride, ferric nitrate, 1,3,5- benzenetricarboxylic acids, hydrofluoric acid are codissolved in water, are put into magnetic stir bar,
Stir at room temperature, take out stirrer, be put into polytetrafluoroethyllining lining, be subsequently placed into reaction kettle, heat up, heat preservation, obtain cobalt/
Iron coordination polymer；
S2, cobalt/iron coordination polymer is calcined in tube furnace ,-three oxygen of cobaltosic oxide is obtained after natural cooling
Change two iron compound oxides；
Wherein, in S1, the time of stirring is 0.5h；
In S1, the temperature of heat preservation is 170 DEG C；
In S1, the time of heat preservation is 72h.
Embodiment 3
A kind of preparation method of cobaltosic oxide-di-iron trioxide composite oxides, includes the following steps：
S1, by cobaltous dichloride, ferric nitrate, 1,3,5- benzenetricarboxylic acids, hydrofluoric acid are codissolved in water, are put into magnetic stir bar,
Stir at room temperature, take out stirrer, be put into polytetrafluoroethyllining lining, be subsequently placed into reaction kettle, heat up, heat preservation, obtain cobalt/
Iron coordination polymer；
S2, cobalt/iron coordination polymer is calcined in tube furnace ,-three oxygen of cobaltosic oxide is obtained after natural cooling
Change two iron compound oxides；
Wherein, in S1, the time of stirring is 3h；
In S1, the temperature of heat preservation is 160 DEG C；
In S1, the time of heat preservation is 80h；
In S2, calcining carries out in the atmosphere of air；
In S2, during calcining, the rate of heating is 1 DEG C/min；
In S2, the temperature of calcining is 600 DEG C；
In S2, the time of calcining is 1h.
Embodiment 4
A kind of preparation method of cobaltosic oxide-di-iron trioxide composite oxides, includes the following steps：
S1, by cobaltous dichloride, ferric nitrate, 1,3,5- benzenetricarboxylic acids, hydrofluoric acid are codissolved in water, are put into magnetic stir bar,
Stir at room temperature, take out stirrer, be put into polytetrafluoroethyllining lining, be subsequently placed into reaction kettle, heat up, heat preservation, obtain cobalt/
Iron coordination polymer；
S2, cobalt/iron coordination polymer is calcined in tube furnace ,-three oxygen of cobaltosic oxide is obtained after natural cooling
Change two iron compound oxides；
Wherein, in S1, the time of stirring is 1h；
In S1, the temperature of heat preservation is 165 DEG C；
In S1, the time of heat preservation is 73h；
In S2, calcining carries out in the atmosphere of air；
In S2, during calcining, the rate of heating is 5 DEG C/min；
In S2, the temperature of calcining is 400 DEG C；
In S2, the time of calcining is 4h；
The cobaltous dichloride, ferric nitrate, 1,3,5- benzenetricarboxylic acids, hydrofluoric acid molar ratio be 2.3：6：2：4；
The molal volume (mmol/ml) of the cobaltous dichloride and water is than being 2.3：40.
Embodiment 5
A kind of preparation method of cobaltosic oxide-di-iron trioxide composite oxides, includes the following steps：
S1, by cobaltous dichloride, ferric nitrate, 1,3,5- benzenetricarboxylic acids, hydrofluoric acid are codissolved in water, are put into magnetic stir bar,
Stir at room temperature, take out stirrer, be put into polytetrafluoroethyllining lining, be subsequently placed into reaction kettle, heat up, heat preservation, obtain cobalt/
Iron coordination polymer；
S2, cobalt/iron coordination polymer is calcined in tube furnace ,-three oxygen of cobaltosic oxide is obtained after natural cooling
Change two iron compound oxides；
Wherein, in S1, the time of stirring is 2h；
In S1, the temperature of heat preservation is 168 DEG C；
In S1, the time of heat preservation is 75h；
In S2, calcining carries out in the atmosphere of air；
In S2, during calcining, the rate of heating is 3 DEG C/min；
In S2, the temperature of calcining is 500 DEG C；
In S2, the time of calcining is 3h；
The cobaltous dichloride, ferric nitrate, 1,3,5- benzenetricarboxylic acids, hydrofluoric acid molar ratio be 2.5：2：5：1；
The molal volume (mmol/ml) of the cobaltous dichloride and water is than being 2.5：35；
The cobaltosic oxide obtained to embodiment 3-5-di-iron trioxide composite oxides carry out SEM detections respectively, as a result
As shown in Figure 1；Wherein, embodiment 4 (a, b), embodiment 5 (c, d), embodiment 3 (e, f).
The cobaltosic oxide obtained to embodiment 3-5-di-iron trioxide composite oxides carry out X-ray diffraction inspection respectively
It surveys, the results are shown in Figure 2.
Test example 1
The cobaltosic oxide that embodiment 3-5 is obtained-di-iron trioxide composite oxides are as active material according to routine
Method is assembled into lithium ion button shape cell respectively, then carries out constant current charge-discharge, test loop service life and high rate performance respectively, knot
Fruit is as shown in Figure 3.
From the figure 3, it may be seen that cobaltosic oxide-di-iron trioxide composite oxides that the present invention is prepared are as electrode material
With higher specific capacity and good cycle performance.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of cobaltosic oxide-di-iron trioxide composite oxides, which is characterized in that include the following steps：
S1, by cobaltous dichloride, ferric nitrate, 1,3,5- benzenetricarboxylic acids, hydrofluoric acid are codissolved in water, stir, heat up, heat preservation, obtain
Cobalt/iron coordination polymer；
S2, cobalt/iron coordination polymer is calcined, cobaltosic oxide-di-iron trioxide composite oxides is obtained after cooling.
2. the preparation method of cobaltosic oxide-di-iron trioxide composite oxides according to claim 1, which is characterized in that
In S1, the time of stirring is 0.5-3h.
3. the preparation method of cobaltosic oxide according to claim 1 or claim 2-di-iron trioxide composite oxides, feature exist
In in S1, the temperature of heat preservation is 160-170 DEG C.
4. special according to the preparation method of any one of the claim 1-3 cobaltosic oxides-di-iron trioxide composite oxides
Sign is, in S1, the time of heat preservation is 72-80h.
5. special according to the preparation method of any one of the claim 1-4 cobaltosic oxides-di-iron trioxide composite oxides
Sign is, in S2, calcining carries out in the atmosphere of air.
6. special according to the preparation method of any one of the claim 1-5 cobaltosic oxides-di-iron trioxide composite oxides
Sign is, in S2, during calcining, the rate of heating is 1-5 DEG C/min.
7. special according to the preparation method of any one of the claim 1-6 cobaltosic oxides-di-iron trioxide composite oxides
Sign is, in S2, the temperature of calcining is 400-500 DEG C.
8. special according to the preparation method of any one of the claim 1-7 cobaltosic oxides-di-iron trioxide composite oxides
Sign is, in S2, the time of calcining is 1-4h.
9. special according to the preparation method of any one of the claim 1-8 cobaltosic oxides-di-iron trioxide composite oxides
Sign is, the cobaltous dichloride, ferric nitrate, 1,3,5- benzenetricarboxylic acids, hydrofluoric acid molar ratio be 2.3-2.5：2-6：2-5：1-
4。
10. according to the preparation method of any one of the claim 1-9 cobaltosic oxides-di-iron trioxide composite oxides,
It is characterized in that, the molal volume (mmol/ml) of the cobaltous dichloride and water is than being 2.3-2.5：35-40.
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2018
- 2018-01-16 CN CN201810039328.2A patent/CN108400318A/en active Pending
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Application publication date: 20180814 |