CN109103431A - A kind of preparation method of sodium ion battery electrode material vanadium phosphate ferrisodium composite material - Google Patents

A kind of preparation method of sodium ion battery electrode material vanadium phosphate ferrisodium composite material Download PDF

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CN109103431A
CN109103431A CN201810944922.6A CN201810944922A CN109103431A CN 109103431 A CN109103431 A CN 109103431A CN 201810944922 A CN201810944922 A CN 201810944922A CN 109103431 A CN109103431 A CN 109103431A
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sodium
ferrisodium
electrode material
vanadium
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王子韩
吕振瑞
张亮
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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
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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

It is an object of the invention to, prepare a kind of sodium-ion battery electrode composite material, it is with preferable performance, and the preparation process of this material is simple, it is low in cost, with good application prospect, mainly there are following steps: 1) being mixed in a certain ratio vanadium source, sodium source, phosphorus source, source of iron uniformly, mixture is placed in progress ball milling initial reaction in high-energy ball milling tank；After, then mixture is transferred in atmosphere furnace and carries out calcination processing, obtain vanadium phosphate ferrisodium electrode material；2) suitable urea is added into vanadium phosphate ferrisodium electrode material obtained above, is mixed uniformly using glass bar, obtain the vanadium phosphate ferrisodium electrode material of N doping as nitrating heat treatment is carried out in tube furnace again after mortar grinder；3) suitable carbon source is added into the vanadium phosphate ferrisodium electrode material of N doping obtained above, is sintered under an inert atmosphere, final product-carbon coating N doping vanadium phosphate ferrisodium electrode material can be obtained.

Description

A kind of preparation method of sodium ion battery electrode material vanadium phosphate ferrisodium composite material
Technical field
The present invention relates to secondary battery positive electrode material preparation fields, and in particular to a kind of electrode material-of sodium-ion battery The preparation method of vanadium phosphate ferrisodium composite material.
Background technique
1997, University of Texas Goodenough et al. disclosed a kind of lithium battery anode material in patent US5910382 Material-LiFePO4 is the one-dimensional tunnel structure material based on olivine structural, has good charge and discharge platform, safety Performance and cycle performance, but since LiFePO4 can only allow lithium ion to move in one direction, and this channel is easily It is influenced and is blocked by impurity in lattice or dislocation, so that the electric conductivity of LiFePO4 and current ratio characteristic are poor, this Outside, in recent years, increasingly rare with lithium mine, so that the cost of this positive electrode also skyrockets therewith.For this reason, it may be necessary to develop one Novel electrode material is planted to solve the problems, such as this, in turn, sodium-ion battery is applied and given birth to.
Sodium-ion battery has the advantage of capacity height and plurality of voltage platforms, for sodium-ion battery, has excellent performance Material be its basic component units, sodium-ion battery has certain requirement to these materials, for example, positive electrode will have height Open-circuit voltage, length cycle life, big reversible capacity；The circulation longevity of security and stability, length that negative electrode material will also have Life, satisfactory reversible capacity, and it is able to carry out quick charge or discharge；Electrolyte require had security and stability, High decomposition voltage, high ionic conductivity, low viscosity coefficient, stable chemical property, resource abundant and cheap Cost etc.；Diaphragm requires have certain ion penetration, and sodium ion is allowed to pass through, and has certain mechanical strength and oxidative resistance Deng.Wherein, electrode is the core component of battery, mainly by groups such as active material, conducting matrix grain, bonding agent and collectors At, directly determine sodium-ion battery energy-storage property quality.
As one kind of sodium-ion battery positive material, vanadium phosphate sodium is since it is with sodium superionic conductors NASICON knot The advantages that structure and good thermal stability, cause extensive research.But the characteristics of vanadium phosphate sodium poorly conductive, so that its multiplying power Poor performance, it is therefore necessary to vanadium phosphate sodium is modified and improve its electric conductivity, to improve its chemical property.Chen etc. People is with " Carbon coated Na3V2(PO4)3 as novel electrode material for sodium ion Batteries " is topic, is modified first using carbon coating to vanadium phosphate ferrisodium in 2012, to greatly improve it Chemical property, voltage is up to 3.4V, specific capacity 93mAh/g.
Summary of the invention
It is an object of the present invention to prepare a kind of sodium-ion battery electrode composite material, with preferable performance, And the preparation process of this material is simple, it is low in cost, with good application prospect.
Sodium-ion battery electrode composite material specifically refers to a kind of carbon-coated N doping vanadium phosphate ferrisodium in the present invention, mark It is denoted as: Na2FeV2(PO4)3-N@C.Na prepared by the present invention2FeV2(PO4)3- N@C electrode material have biggish specific surface area and Pore structure abundant, this is conducive to electrode material and the infiltration of electrolyte and contacts, and when being assembled into battery, shows very well Chemical property, meanwhile, the material is steady with good electric conductivity and structure due to the codope component with carbon and nitrogen It is qualitative, compared with the electrode material not being modified, show higher charge/discharge capacity and better cyclical stability.
Specifically, the purpose of the present invention is realized by the following method:
A kind of preparation method of sodium ion battery electrode material vanadium phosphate ferrisodium composite material:
1) vanadium source, sodium source, phosphorus source, source of iron are mixed in a certain ratio uniformly, mixture is placed in high-energy ball milling tank and carries out ball Grind initial reaction；After, then mixture is transferred in atmosphere furnace and carries out calcination processing, obtain vanadium phosphate ferrisodium electrode material Material；
2) suitable urea is added into vanadium phosphate ferrisodium electrode material obtained above, is mixed uniformly using glass bar, The vanadium phosphate ferrisodium electrode material of N doping is obtained as nitrating heat treatment is carried out in tube furnace again after mortar grinder；
3) suitable carbon source is added into the vanadium phosphate ferrisodium electrode material of N doping obtained above, carries out under an inert atmosphere Sintering, can be obtained final product-carbon coating N doping vanadium phosphate ferrisodium electrode material.
Further, vanadium source is selected from vanadic anhydride, two sodium vanadates, ammonium metavanadate, vanadium dioxide, dioxy chlorine in step 1) One or more of vanadium；Sodium source is selected from sodium carbonate, sodium citrate, sodium dihydrogen phosphate, sodium alginate, sodium hydroxide, bicarbonate One or more of sodium；Source of iron is selected from one or more of FeO, ferric nitrate, ferric acetyl acetonade；Phosphorus source is selected from phosphoric acid, phosphorus One or more of acid dihydride ammonium, diammonium hydrogen phosphate, sodium dihydrogen phosphate.
Further, in step 1) according to vanadium ion, sodium ion, iron ion and phosphorus in vanadium source, sodium source, source of iron and phosphorus source from Sub- molar ratio is that 2.0:2.0:1.0:3 weighs the vanadium source, sodium source, source of iron and phosphorus source.
Further, the reaction of high-energy ball milling tank described in step 1) difference and general ball milling, are not only simple Mixed grinding, but make that preliminary reaction occurs between reactant, generate presoma, the high-energy ball milling condition are as follows: ball material Than for 10-15:1, rotational speed of ball-mill 500-1000rpm, Ball-milling Time 5-10min.
Further, calcination processing described in step 1), which refers to, is heat-treated 8- at 800-900 DEG C under an inert atmosphere 12h。
Further, the processing of nitrating described in step 2 refers to first carries out nitrating processing for mixture at 150 DEG C, so 800 DEG C are warming up to the speed of 5-12 DEG C/min again afterwards, on the one hand reacts reactant further, on the other hand, is removed not anti- The urea answered.
Further, carbon source described in step 3) refers to one of glucose, citric acid or sucrose；The sintering Condition, which refers to, is sintered 5-8h at 550 DEG C.
The sodium ion battery electrode material prepared by the above method.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention introduces nitrogen in vanadium phosphate ferrisodium electrode material for the first time, and is realized instead using the mode of high-energy ball milling The initial reaction of raw material is answered, this has apparent influence to the final performance of material；By the way that the electrode material is applied to sodium ion Battery, it is found that its capacity under the current density of 30C can achieve 109.8mAh/g, the capacity under the current density of C/50 It can achieve 143.3mAh/g.Preferable volumetric properties are shown, and at higher current densities, also shows and follow well Ring stability, this all proves that this material is a kind of sodium ion battery electrode material with very high potential.
Detailed description of the invention
The stereoscan photograph of Fig. 1 product prepared by the present invention；
The battery performance test map of Fig. 2 electrode material prepared by the present invention.
Specific embodiment
Embodiment 1
It is 2.0:2.0 according to vanadium ion, sodium ion, iron ion and phosphonium ion molar ratio in vanadium source, sodium source, source of iron and phosphorus source: 1.0:3 weighs vanadic anhydride, sodium carbonate, FeO and ammonium dihydrogen phosphate, will be placed on high energy after above-mentioned load weighted material mixing In ball grinder, using zirconium oxide as mill ball, taken out after grinding 10min at 800 rpm；Then by it under argon atmosphere in 800 DEG C sintering 10h；Suitable urea is weighed again afterwards to be mixed with preceding product, first at 150 DEG C carry out nitrating processing, after again with The heating rate of 5 DEG C/min is warming up to 800 DEG C and carries out heat preservation heat treatment 2h；After reaction, be down to room temperature to product, then to its It is middle to be added after suitable glucose is stirred, 6h is sintered at 550 DEG C, after sintering, by final product use go from Sub- water and ethyl alcohol repeatedly wash.
Embodiment 2
It is 2.0:2.0 according to vanadium ion, sodium ion, iron ion and phosphonium ion molar ratio in vanadium source, sodium source, source of iron and phosphorus source: 1.0:3 weighs vanadium dioxide, sodium hydroxide, ferric nitrate and diammonium hydrogen phosphate, will be placed on after above-mentioned load weighted material mixing In high-energy ball milling tank, using zirconium oxide as mill ball, taken out after grinding 10min at 800 rpm；Then by it under argon atmosphere In 800 DEG C of sintering 10h；It weighs suitable urea again afterwards to be mixed with preceding product, nitrating processing is first carried out at 150 DEG C, 800 DEG C, which are warming up to, with the heating rate of 5 DEG C/min again afterwards carries out heat preservation heat treatment 2h；After reaction, it is down to room temperature to product, It is added thereto after suitable sucrose is stirred again, 6h is sintered at 550 DEG C, after sintering, final product is used Deionized water and ethyl alcohol repeatedly wash.
Embodiment 3
It is 2.0:2.0 according to vanadium ion, sodium ion, iron ion and phosphonium ion molar ratio in vanadium source, sodium source, source of iron and phosphorus source: 1.0:3 weighs vanadium dioxide, sodium hydroxide and sodium citrate, ferric nitrate and diammonium hydrogen phosphate, and above-mentioned load weighted substance is mixed It is placed on after conjunction in high-energy ball milling tank, using zirconium oxide as mill ball, is taken out after grinding 8min at 1000rpm；Then by its In 800 DEG C of sintering 10h under nitrogen atmosphere；It weighs suitable urea again afterwards to be mixed with preceding product, first be carried out at 150 DEG C Nitrating processing, after again with the heating rate of 10 DEG C/min be warming up to 800 DEG C carry out heat preservation heat treatment 2h；After reaction, wait produce Object is down to room temperature, then is added after suitable glucose is stirred thereto, and 6h is sintered at 550 DEG C, will most after sintering Whole product is repeatedly washed using deionized water and ethyl alcohol.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from invention Design or beyond the scope defined by this claim, be within the scope of protection of the invention.

Claims (9)

1. a kind of preparation method of sodium ion battery electrode material vanadium phosphate ferrisodium composite material, it is characterised in that: including following Step:
1) vanadium source, sodium source, phosphorus source, source of iron are mixed in a certain ratio uniformly, mixture is placed in high-energy ball milling tank and carries out ball Grind initial reaction；After, then mixture is transferred in atmosphere furnace and carries out calcination processing, obtain vanadium phosphate ferrisodium electrode material Material；
2) suitable urea is added into vanadium phosphate ferrisodium electrode material obtained above, is mixed uniformly using glass bar, The vanadium phosphate ferrisodium electrode material of N doping is obtained as nitrating heat treatment is carried out in tube furnace again after mortar grinder；
3) suitable carbon source is added into the vanadium phosphate ferrisodium electrode material of N doping obtained above, carries out under an inert atmosphere Sintering, can be obtained final product-carbon coating N doping vanadium phosphate ferrisodium electrode material.
2. a kind of preparation method of sodium ion battery electrode material vanadium phosphate ferrisodium composite material according to claim 1, It is characterized by: vanadium source is in vanadic anhydride, two sodium vanadates, ammonium metavanadate, vanadium dioxide, dioxy chlorine vanadium in step 1) It is one or more of；Sodium source is in sodium carbonate, sodium citrate, sodium dihydrogen phosphate, sodium alginate, sodium hydroxide, sodium bicarbonate It is one or more of；Source of iron is selected from one or more of FeO, ferric nitrate, ferric acetyl acetonade；Phosphorus source is selected from phosphoric acid, biphosphate One or more of ammonium, diammonium hydrogen phosphate, sodium dihydrogen phosphate.
3. a kind of preparation method of sodium ion battery electrode material vanadium phosphate ferrisodium composite material according to claim 1, It is characterized by: according to vanadium ion, sodium ion, iron ion and phosphonium ion mole in vanadium source, sodium source, source of iron and phosphorus source in step 1) Than weighing the vanadium source, sodium source, source of iron and phosphorus source for 2.0:2.0:1.0:3.
4. a kind of preparation method of sodium ion battery electrode material vanadium phosphate ferrisodium composite material according to claim 1, It is characterized by: high-energy ball milling condition described in step 1) are as follows: ratio of grinding media to material 10-15:1, rotational speed of ball-mill 500- 1000rpm, Ball-milling Time 5-10min.
5. a kind of preparation method of sodium ion battery electrode material vanadium phosphate ferrisodium composite material according to claim 1, It is characterized by: calcination processing described in step 1), which refers to, is heat-treated 8-12h at 800-900 DEG C under an inert atmosphere.
6. a kind of preparation method of sodium ion battery electrode material vanadium phosphate ferrisodium composite material according to claim 1, It is characterized by: nitrating described in step 2 processing refer to by mixture first at 150 DEG C carry out nitrating processing, then again with The speed of 5-12 DEG C/min is warming up to 800 DEG C, on the one hand reacts reactant further, on the other hand, removes unreacted urine Element.
7. a kind of preparation method of sodium ion battery electrode material vanadium phosphate ferrisodium composite material according to claim 1, It is characterized by: carbon source described in step 3) refers to one of glucose, citric acid or sucrose；The sintering condition is Finger is sintered 5-8h at 550 DEG C.
8. the carbon coating N doping vanadium phosphate ferrisodium electrode material of -7 either method preparation according to claim 1.
9. electrode material is applied to sodium-ion battery according to claim 8.
CN201810944922.6A 2018-08-19 2018-08-19 A kind of preparation method of sodium ion battery electrode material vanadium phosphate ferrisodium composite material Withdrawn CN109103431A (en)

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Cited By (6)

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CN110085862A (en) * 2019-04-26 2019-08-02 北京金羽新能科技有限公司 A kind of sode cell electrode material Na1+xFexTi2-x(PO4)3And its preparation method and application
CN110993942A (en) * 2020-01-02 2020-04-10 同济大学 High-performance sodium-deficient cathode material and sodium-ion battery
CN114204030A (en) * 2021-12-02 2022-03-18 南昌大学 Modification method of lithium ferric manganese phosphate positive electrode material
CN114725345A (en) * 2022-04-19 2022-07-08 江苏理工学院 Fe3O4/NaTi2(PO4)3Preparation method and application of/C micro-nano composite material
CN114759173A (en) * 2022-03-21 2022-07-15 上海电力大学 Trivalent chromium ion doped modified mixed ferric sodium pyrophosphate positive electrode material, preparation and application
CN115304046A (en) * 2022-09-08 2022-11-08 四川大学 Sodium vanadium phosphate, sodium vanadium manganese phosphate and preparation method thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110085862A (en) * 2019-04-26 2019-08-02 北京金羽新能科技有限公司 A kind of sode cell electrode material Na1+xFexTi2-x(PO4)3And its preparation method and application
CN110993942A (en) * 2020-01-02 2020-04-10 同济大学 High-performance sodium-deficient cathode material and sodium-ion battery
CN114204030A (en) * 2021-12-02 2022-03-18 南昌大学 Modification method of lithium ferric manganese phosphate positive electrode material
CN114759173A (en) * 2022-03-21 2022-07-15 上海电力大学 Trivalent chromium ion doped modified mixed ferric sodium pyrophosphate positive electrode material, preparation and application
CN114725345A (en) * 2022-04-19 2022-07-08 江苏理工学院 Fe3O4/NaTi2(PO4)3Preparation method and application of/C micro-nano composite material
CN115304046A (en) * 2022-09-08 2022-11-08 四川大学 Sodium vanadium phosphate, sodium vanadium manganese phosphate and preparation method thereof

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