CN107200358A - A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material - Google Patents
A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material Download PDFInfo
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- CN107200358A CN107200358A CN201710274653.2A CN201710274653A CN107200358A CN 107200358 A CN107200358 A CN 107200358A CN 201710274653 A CN201710274653 A CN 201710274653A CN 107200358 A CN107200358 A CN 107200358A
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- cufe
- sodium
- iron system
- ion battery
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000000463 material Substances 0.000 title claims abstract description 63
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910001415 sodium ion Inorganic materials 0.000 title claims abstract description 37
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 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 30
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002671 adjuvant Substances 0.000 claims abstract description 17
- 238000002485 combustion reaction Methods 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 24
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 12
- 239000004471 Glycine Substances 0.000 claims description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 12
- 239000002086 nanomaterial Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 239000007790 solid phase Substances 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 238000007796 conventional method Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract description 2
- 230000036632 reaction speed Effects 0.000 abstract description 2
- 238000011017 operating method Methods 0.000 abstract 1
- 229910016516 CuFe2O4 Inorganic materials 0.000 description 16
- 239000007772 electrode material Substances 0.000 description 14
- 230000002441 reversible effect Effects 0.000 description 13
- 239000011734 sodium Substances 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- KBIWNQVZKHSHTI-UHFFFAOYSA-N 4-n,4-n-dimethylbenzene-1,4-diamine;oxalic acid Chemical compound OC(=O)C(O)=O.CN(C)C1=CC=C(N)C=C1 KBIWNQVZKHSHTI-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229910000528 Na alloy Inorganic materials 0.000 description 1
- 229910014537 Na0.7CoO2 Inorganic materials 0.000 description 1
- 229910020657 Na3V2(PO4)3 Inorganic materials 0.000 description 1
- 229910021312 NaFePO4 Inorganic materials 0.000 description 1
- 229910019398 NaPF6 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Natural products OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 229920000447 polyanionic polymer Polymers 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000002226 superionic conductor Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/0018—Mixed oxides or hydroxides
- C01G49/0081—Mixed oxides or hydroxides containing iron in unusual valence state [IV, V, VI]
-
- 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
-
- 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
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
-
- 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
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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 iron system CuFe for sodium-ion battery2O4The preparation method of material, belongs to materials synthesis and energy technology field.Copper nitrate, ferric nitrate, combustion adjuvant are dissolved into deionized water by the present invention obtains mixed solution, and under the conditions of temperature is 80 ~ 100 DEG C, mixed solution is dried to obtain into gel, 200 ~ 300 DEG C and 1 ~ 15min of constant temperature are again heated to；Product high-temperature calcination is produced into the iron system CuFe for sodium-ion battery2O4Material.The present invention prepares iron system CuFe using micro-gel flooding2O4Material, it is to avoid the operating procedure of solid-phase grinding in conventional method, is conducive to accelerating reaction speed, shortens the reaction time, improves the uniformity of product physicochemical property, the material of preparation is micro-nano structure, can both accelerate the transmission of sodium ion electronics, improves electro-chemical activity；The stability of material can be increased again, the machinability and storage stability of material is improved.
Description
Technical field
The present invention relates to a kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, belong to materials synthesis and
Energy technology field.
Background technology
At present, lithium ion battery is development prospect the brightest and the clearest high-energy battery system, but with industries such as number, traffic
Lithium ion battery is relied on and aggravated, limited lithium resource will face shortage problem.Sodium compares lithium resource as common elements, reserves
High several orders of magnitude, account for the 2.64% of the earth's crust, and be evenly distributed, it is easy to refine.Therefore, sodium-ion battery is that a kind of pole has
The secondary cell of development potentiality.Common sodium-ion battery positive material mainly has oxide type such as Na0.7CoO2, polyanion
Type such as NaFePO4With sodium superionic conductors material such as Na3V2(PO4)3Deng；The main carbon-based material of negative material such as petroleum coke, titanium-based
Material such as TiO2With sodium alloy material etc., and ferrite sodium-ion battery negative pole not yet has been reported that.
Existing iron system CuFe2O4After the preparation method of material is mixed with solid-phase ball milling, then it is placed in 900~1100 DEG C of bars of high temperature
Calcine and be made under part, material physicochemical property prepared by this method is uneven and is easy to reunite, so as to be unfavorable for its commercialization
Production.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of iron system CuFe for sodium-ion battery2O4The preparation of material
Method, i.e., using gel-combustion method one-step synthesis material, shorten the reaction time, improve the uniformity of product physicochemical property, prepare
Material be micro-nano structure, can both accelerate the transmission of sodium ion electronics, improve electro-chemical activity；The steady of material can be increased again
It is qualitative, improve the machinability and storage stability of material.
A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, is comprised the following steps that：
（1）Copper nitrate, ferric nitrate, combustion adjuvant are dissolved into deionized water and obtain mixed solution, is 80 ~ 100 DEG C of bars in temperature
Under part, mixed solution is dried to obtain gel, 200 ~ 300 DEG C and the min of constant temperature 1 ~ 15 are then again heated to；
（2）By step（1）Products therefrom progress high-temperature calcination produces the iron system CuFe for sodium-ion battery2O4Material；
The step（1）The mol ratio of middle copper nitrate and ferric nitrate is 1:2, the mol ratio of combustion adjuvant and copper nitrate is 1:1~1:6；
The step（1）Middle combustion adjuvant is one kind or any than a variety of in glycine, citric acid, sucrose, glucose；
The step（2）The temperature of high temperature calcining is 700 ~ 900 DEG C, and the time is 0.5 ~ 5h.
Beneficial effects of the present invention：
（1）The present invention prepares iron system CuFe using gel-combustion method2O4Material, it is to avoid the behaviour of solid-phase grinding in conventional method
Make step, be conducive to accelerating reaction speed, shorten the reaction time；
（2）Electrode material prepared by the inventive method has porous micro-nano structure, and nanostructured therein not only improves electrolyte
Infiltration, be conducive to the electronics of electrolysis material to transmit with sodium ion again to improve the chemical property of material；Micrometer structure is then
Increase the stability that material is prepared, stored, production and storage cost are reduced to a certain extent；
（3）CuFe of the present invention2O4Electrode material has stronger cycle performance, CuFe2O4Under 200mA/g high current density
The reversible capacity that circulation is 50 times can reach more than 300mAh/g.
Brief description of the drawings
Fig. 1 is CuFe prepared by the embodiment of the present invention 12O4The XRD of material；
Fig. 2 is CuFe prepared by the embodiment of the present invention 12O4The SEM figures of material；
Fig. 3 is CuFe prepared by the embodiment of the present invention 12O4The chemical property figure of material；
Fig. 4 is CuFe prepared by the embodiment of the present invention 22O4The chemical property figure of material；
Fig. 5 is CuFe prepared by the embodiment of the present invention 32O4The chemical property figure of material；
Fig. 6 is CuFe prepared by the embodiment of the present invention 42O4The chemical property figure of material；
Fig. 7 is CuFe prepared by the embodiment of the present invention 52O4The chemical property figure of material；
Fig. 8 is the chemical property figure of comparative example.
Embodiment
The present invention is described in further detail with reference to embodiment, but protection scope of the present invention is not limited
In the content.
Embodiment 1：A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, is comprised the following steps that：
（1）By copper nitrate, ferric nitrate, combustion adjuvant（Citric acid）It is dissolved into deionized water and obtains mixed solution, wherein copper nitrate
Mol ratio with ferric nitrate is 1:2, combustion adjuvant（Citric acid）Mol ratio with copper nitrate is 1:3, under the conditions of temperature is 90 DEG C,
Mixed solution is dried to obtain gel, is then placed in again in electric furnace and is heated to 240 DEG C and the min of constant temperature 5；
（2）By step（1）Products therefrom progress high-temperature calcination produces the iron system CuFe for sodium-ion battery2O4Material, wherein
The temperature of high-temperature calcination is 800 DEG C, and the time is 2h；
CuFe manufactured in the present embodiment2O4The XRD of material is as shown in figure 1, from fig. 1, it can be seen that the CuFe2O4Material crystal structure
For spinel structure and no impurity, CuFe manufactured in the present embodiment2O4The SEM of material is schemed as shown in Fig. 2 can from Fig. 2
Know, the CuFe2O4The microstructure of material is porous micro-nano structure particle, and particle diameter is 80 ~ 220nm；
Electrochemical property test：By the CuFe obtained by the present embodiment2O4Material, acetylene black and sodium carboxymethylcellulose（CMC）
In mass ratio 8:1 :1 is well mixed, and adds appropriate amount of deionized water dissolving, slurry film is made into electrode on copper foil.By this
Test electrode 110 DEG C of dryings 24 hours in vacuum drying oven, with EC/DEC=1 in high-purity argon atmosphere glove box：1（Volume
Than）With NaPF6For electrolyte, using glass fiber filter paper as barrier film, metallic sodium is that GND is assembled into button battery.Put and fill
Electric condition：Discharged into identical current density and 3V is recharged to after 0.02V, the current density of selection is 200mA/g.To above-mentioned
Battery carries out electro-chemical test, and test result is as shown in figure 3, from the figure 3, it may be seen that CuFe2O4Electrode material is close in 200mA/g electric currents
The lower discharge and recharge of degree, reversible capacity is maintained at 320.6 mAh/g after circulating 50 times.
Embodiment 2：A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, is comprised the following steps that：
（1）By copper nitrate, ferric nitrate, combustion adjuvant（Glycine）It is dissolved into deionized water and obtains mixed solution, wherein copper nitrate
Mol ratio with ferric nitrate is 1:2, combustion adjuvant（Glycine）Mol ratio with copper nitrate is 1:2, under the conditions of temperature is 80 DEG C,
Mixed solution is dried to obtain gel, is then placed in again in electric furnace and is heated to 270 DEG C and the min of constant temperature 7；
（2）By step（1）Products therefrom progress high-temperature calcination produces the iron system CuFe for sodium-ion battery2O4Material, wherein
The temperature of high-temperature calcination is 700 DEG C, and the time is 4.5h；
Electrochemical property test：The electrochemical property test of the present embodiment is same as Example 1, test result as shown in figure 4, by
Knowable to Fig. 4, CuFe2O4Electrode material discharge and recharge under 200mA/g current densities, reversible capacity is maintained at 247 after circulating 50 times
mAh/g。
Embodiment 3：A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, is comprised the following steps that：
（1）By copper nitrate, ferric nitrate, combustion adjuvant（Citric acid）It is dissolved into deionized water and obtains mixed solution, wherein copper nitrate
Mol ratio with ferric nitrate is 1:2, combustion adjuvant（Citric acid）Mol ratio with nitrate is 1:4, it is 100 DEG C of conditions in temperature
Under, mixed solution is dried to obtain gel, is then placed in again in electric furnace and is heated to 250 DEG C and the min of constant temperature 9；
（2）By step（1）Products therefrom progress high-temperature calcination produces the iron system CuFe for sodium-ion battery2O4Material, wherein
The temperature of high-temperature calcination is 900 DEG C, and the time is 2.5h；
Electrochemical property test：The electrochemical property test of the present embodiment is same as Example 1, test result as shown in figure 5, by
Knowable to Fig. 5, CuFe2O4Electrode material discharge and recharge under 200mA/g current densities, reversible capacity is maintained at 187.6 after circulating 50 times
mAh/g。
Embodiment 4：A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, is comprised the following steps that：
（1）By copper nitrate, ferric nitrate, combustion adjuvant（Glucose）It is dissolved into deionized water and obtains mixed solution, wherein copper nitrate
Mol ratio with ferric nitrate is 1:2, combustion adjuvant（Glucose）Mol ratio with copper nitrate is 1:1, under the conditions of temperature is 85 DEG C,
Mixed solution is dried to obtain gel, is then placed in again in electric furnace and is heated to 220 DEG C and the min of constant temperature 12；
（2）By step（1）Products therefrom progress high-temperature calcination produces the iron system CuFe for sodium-ion battery2O4Material, wherein
The temperature of high-temperature calcination is 750 DEG C, and the time is 3.5h；
Electrochemical property test：The electrochemical property test of the present embodiment is same as Example 1, test result as shown in fig. 6, by
Knowable to Fig. 6, CuFe2O4Electrode material discharge and recharge under 200mA/g current densities, reversible capacity is maintained at 191.3 after circulating 50 times
mAh/g。
Embodiment 5：A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, is comprised the following steps that：
（1）By copper nitrate, ferric nitrate, combustion adjuvant（The mixture of glycine and citric acid）It is dissolved into deionized water and is mixed
The mol ratio of solution, wherein copper nitrate and ferric nitrate is 1:2, combustion adjuvant（The mixture of glycine and citric acid）With copper nitrate
Mol ratio is 1:6, under the conditions of temperature is 85 DEG C, mixed solution is dried to obtain gel, is then placed in electric furnace and is heated to again
280 DEG C and the min of constant temperature 3；
（2）By step（1）Products therefrom progress high-temperature calcination produces the iron system CuFe for sodium-ion battery2O4Material, wherein
The temperature of high-temperature calcination is 850 DEG C, and the time is 2.8h；
Electrochemical property test：The electrochemical property test of the present embodiment is same as Example 1, test result as shown in fig. 7, by
Knowable to Fig. 7, CuFe2O4Electrode material discharge and recharge under 200mA/g current densities, reversible capacity is maintained at 218.9 after circulating 50 times
mAh/g。
Embodiment 6：A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, is comprised the following steps that：
Step is substantially the same manner as Example 1, is a difference in that step（1）Middle electric furnace heating-up temperature is 200 DEG C.Chemical property is surveyed
Test result shows, CuFe2O4Electrode material discharge and recharge under 200mA/g current densities, reversible capacity is maintained at after circulating 50 times
298.5mAh/g。
Embodiment 7：A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, is comprised the following steps that：
Step is substantially the same manner as Example 1, simply step（1）Middle electric furnace heating-up temperature is 300 DEG C.Electrochemical property test result
It has been shown that, CuFe2O4Electrode material discharge and recharge under 200mA/g current densities, reversible capacity is maintained at 287.5 after circulating 50 times
mAh/g。
Embodiment 8：A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, is comprised the following steps that：
Step is substantially the same manner as Example 1, is a difference in that step（1）The middle electric furnace heat time is 1 min.Chemical property is surveyed
Test result shows, CuFe2O4Electrode material discharge and recharge under 200mA/g current densities, reversible capacity is maintained at after circulating 50 times
310.5 mAh/g。
Embodiment 9：A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, is comprised the following steps that：
Step is substantially the same manner as Example 1, is a difference in that step（1）The middle electric furnace heat time is 15 min.Chemical property
Test result shows, CuFe2O4Electrode material discharge and recharge under 200mA/g current densities, reversible capacity is maintained at after circulating 50 times
305.7mAh/g。
Embodiment 10：A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, is comprised the following steps that：
Step is substantially the same manner as Example 1, is a difference in that step（2）Middle calcination time is 0.5 h.Electrochemical property test knot
Fruit display, CuFe2O4Electrode material discharge and recharge under 200mA/g current densities, reversible capacity is maintained at after circulating 50 times
305.7mAh/g。
Embodiment 11：A kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, is comprised the following steps that：
Step is substantially the same manner as Example 1, is a difference in that step（2）Middle calcination time is 5 h.Electrochemical property test result
It has been shown that, CuFe2O4Electrode material discharge and recharge under 200mA/g current densities, reversible capacity is maintained at after circulating 50 times
305.7mAh/g。
Comparative example：Coprecipitation prepares the iron system CuFe of sodium-ion battery2O4Material, is comprised the following steps that：
（1）The CuSO that 60 ml concentration are 0.1mol/L is added into beaker4Solution, 120 ml concentration are 0.1mol/L FeSO4
Solution and 180 ml ethanol, it is well mixed to obtain mixed solution；
（2）At ambient temperature, in step（1）The ethanedioic acid that 185 ml concentration are 0.1mol/L is added in middle gained mixed solution
Sodium（Na2C2O4）Solution simultaneously reacts 3 h under the conditions of magnetic agitation, filters, dries；
（3）By step（2）Products therefrom is calcined, wherein the temperature calcined is 400 DEG C, the time is that 10 min obtain sodium ion
The iron system CuFe of battery2O4Material；
Electrochemical property test：The electrochemical property test of the present embodiment is same as Example 1, test result as shown in figure 8, by
Knowable to Fig. 7, CuFe2O4Electrode material discharge and recharge under 200mA/g current densities, reversible capacity is maintained at after circulating 50 times
212.1mAh/g。
Claims (4)
1. a kind of iron system CuFe for sodium-ion battery2O4The preparation method of material, it is characterised in that comprise the following steps that：
（1）Copper nitrate, ferric nitrate, combustion adjuvant are dissolved into deionized water and obtain mixed solution, is 80 ~ 100 DEG C of bars in temperature
Under part, mixed solution is dried to obtain gel, 200 ~ 300 DEG C and 1 ~ 15min of constant temperature are then again heated to；
（2）By step（1）Products therefrom progress high-temperature calcination produces the iron system CuFe for sodium-ion battery2O4Material.
2. it is used for the iron system CuFe of sodium-ion battery according to claim 12O4The preparation method of material, it is characterised in that：Step
Suddenly（1）The mol ratio of middle copper nitrate and ferric nitrate is 1:2, the mol ratio of combustion adjuvant and copper nitrate is 1:1~1:6.
3. it is used for the iron system CuFe of sodium-ion battery according to claim 12O4The preparation method of material, it is characterised in that：Step
Suddenly（1）Middle combustion adjuvant is one kind or any than a variety of in glycine, citric acid, sucrose, glucose.
4. it is used for the iron system CuFe of sodium-ion battery according to claim 12O4The preparation method of material, it is characterised in that：Step
Suddenly（2）The temperature of high temperature calcining is 700 ~ 900 DEG C, and the time is 0.5 ~ 5h.
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| CN108400299A (en) * | 2018-02-08 | 2018-08-14 | 江西理工大学 | A kind of preparation method of CuFe2O4/C composite negative pole materials for sodium-ion battery |
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