CN108807906A - A kind of preparation method of nitrogen-doped carbon cladding classification through-hole structure ferroferric oxide composite cathode material - Google Patents

A kind of preparation method of nitrogen-doped carbon cladding classification through-hole structure ferroferric oxide composite cathode material Download PDF

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CN108807906A
CN108807906A CN201810602319.XA CN201810602319A CN108807906A CN 108807906 A CN108807906 A CN 108807906A CN 201810602319 A CN201810602319 A CN 201810602319A CN 108807906 A CN108807906 A CN 108807906A
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classification
hole structure
nitrogen
oxide composite
ferroferric oxide
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CN108807906B (en
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武大鹏
陈俊良
任好雨
刘宁
曹锟
徐芳
高志永
蒋凯
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Henan Normal University
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    • 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
    • H01M10/052—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
    • 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
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    • H01M4/625—Carbon or graphite
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses the preparation methods that a kind of nitrogen-doped carbon coats classification through-hole structure ferroferric oxide composite cathode material, belong to the synthesis technical field of inorganic functional material.Technical scheme of the present invention main points are：Using hydro-thermal etching method to cubical α-Fe2O3It is etched, the α-Fe with classification through-hole structure has been obtained after being etched along body-centered direction2O3The volume expansion of material is alleviated in cube, the presence of through-hole structure, while improving the kinetics of diffusion process of electrolyte, then by carbon coating and has been thermally treated resulting in the carbon-coated classification through-hole ferroferric oxide composite cathode material Fe of N doping3O4@N-C increase the electric conductivity and stability of material.Meanwhile by having obtained the composite material that structure has good stability to the regulation and control of acid concentration in etching process, further improving the stable circulation performance of electrode material.

Description

A kind of nitrogen-doped carbon cladding classification through-hole structure ferroferric oxide composite cathode material Preparation method
Technical field
The invention belongs to the synthesis technical fields of inorganic functional material, and in particular to a kind of nitrogen-doped carbon cladding classification through-hole The preparation method of structure ferroferric oxide composite cathode material.
Background technology
Under the challenge of global energy crisis and environmental crisis, exploitation and the environmental improvement of new energy are particularly important, Cheap, environmentally friendly, the efficient material of synthesis is simultaneously applied in practice, is the effective way for solving energy and environmental problem.With business stone Ink is compared, and transition metal oxide usually has higher theoretical capacity, therefore transition metal oxide is before a kind of comparison has The substitute of scape.
Fe3O4It is an important member in transition metal oxide family, theoretical capacity is up to 926 mAh g-1。Fe3O4 Since many features of itself are such as enriched, voluminous, inexpensive, nontoxic, synthesis technology is simple and has good stability, and becomes one The good lithium ion battery negative material of kind.But metal oxide is frequently run onto in the application process of lithium cell negative pole material Some are difficult to overcome the problems, such as, such as poor electric conductivity, the loss of higher initial capacity and larger volume change.Wherein, Fe3O4The volume expansion generated in charge and discharge process is to limit the principal element of the materials industrialization.Although vast research work Person has done a large amount of investigation and comparison to its pattern, size, to a certain extent so that cyclical stability is improved, but still So it is difficult to meet the needs of people.It is negative that the patent of Publication No. CN 103227324A discloses a kind of lithium ion battery iron oxide The preparation method of pole material, in 0.1 A g-1Current density under, reversible capacity is only protected after 20 charge and discharge cycles It holds in 454.8 mAh g-1.The patent of Publication No. CN 106450189A discloses the carbon coating iron oxide cathode with N doping Material, under 1C multiplying powers, initial reversible discharge specific capacity only has 647 mAh g-1, after cycle 100 is enclosed, capacity only has 624 mAh g-1。
Invention content
The technical problem to be solved by the present invention is to provide a kind of simple for process and low-cost nitrogen-doped carbon claddings to be classified The preparation method of through-hole ferroferric oxide composite cathode material, composite negative pole material made from this method is carved by using hydro-thermal Erosion method is to cubical α-Fe2O3It performs etching, porous α-Fe is obtained after being etched along body-centered direction2O3Cube, then By carbon coating and it is thermally treated resulting in the carbon-coated Fe of N doping3O4@N-C composite negative pole materials, are effectively increased the conduction of material Property, while by having obtained the composite negative pole material that structure has good stability to the regulation and control of acid concentration in etching process, further Improve the stable circulation performance of electrode material.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, a kind of nitrogen-doped carbon cladding classification through-hole structure The preparation method of ferroferric oxide composite cathode material, it is characterised in that the specific steps are：
（1）By 0.1 g α-Fe2O3It is 0.2~0.6 mol L to be added to 30 mL molar concentrations-1Hydrochloric acid solution in, stirring 5 Mixed solution is transferred in polytetrafluoro reaction kettle and in 160 DEG C of 12 h of hydro-thermal reaction, is centrifuged after being cooled to room temperature, by institute by min Obtained red precipitate deionized water and ethyl alcohol difference rinse 3 times, the α-of etching processing is obtained then at 60 DEG C of dry 2 h Fe2O3；
（2）By the α-Fe of 0.3 g etching processings2O3It is added in the Tris solution that 150mL molar concentrations are 10 mM, stirring 10 Min is added 0.15 g Dopamine hydrochlorides, stirs 6 h under room temperature, 3 are washed with deionized water and ethyl alcohol respectively after solution is centrifuged It is secondary, the sample of cladding dopamine is obtained then at 60 DEG C of dry 2 h, is then dried overnight, the product that will be obtained in a nitrogen environment 2~4 h are calcined in 500~600 DEG C obtains nitrogen-doped carbon cladding classification through-hole structure ferroferric oxide composite cathode material Fe3O4@ N-C。
Further preferably, step（1）Described in the molar concentration of hydrochloric acid solution be preferably 0.4 mol L-1。
The present invention has the advantages that compared with prior art：The present invention is using hydro-thermal etching method to cubical α- Fe2O3It performs etching, the α-Fe of multistage through-hole structure is obtained after being etched along body-centered direction2O3, the presence raising of through-hole structure Link of the material to volume expansion, while improving the kinetics of diffusion process of electrolyte.By carbon coating and it is heat-treated To the carbon-coated classification through-hole structure ferroso-ferric oxide Fe of N doping3O4@N-C increase the electric conductivity of material.Meanwhile by right The regulation and control of acid concentration have obtained the composite material that structure has good stability in etching process, and the cycle for further improving electrode is steady Qualitative energy.
Description of the drawings
Fig. 1 is α-Fe2O3（A, b）And different acidity is to α-Fe2O3Pattern after progress hydro-thermal etching（α-Fe2O3-0.2（C, d）,α-Fe2O3-0.4（E, f）,α-Fe2O3-0.6（G, h））SEM figure；
Fig. 2 is α-Fe2O3In N2α-the Fe obtained after being calcined under environment2O3-500（a-c）, to untreated α-Fe2O3And warp Cross the α-Fe of hydro-thermal etching2O3The SEM figures that pattern changes after carrying out packet carbon and calcining（（Fe3O4@N-C）（d-f）,Fe3O4-0.2@ N-C（g-i）,Fe3O4-0.4@N-C（j-l),Fe3O4-0.6@N-C（m-o））；
Fig. 3 is α-Fe2O3-0.4、α-Fe2O3-500、Fe3O4@N-C、Fe3O4-0.2@N-C、Fe3O4-0.4@N-C、Fe3O4-0.6@ The XRD diagram of N-C；
Fig. 4 is untreated α-Fe2O3（a）,α-Fe2O3-0.4（b）And Fe3O4-0.4@N-C（c）TEM and to single Fe3O4-0.4@N-C（d）Mapping analysis（e-h）Figure；
Fig. 5 is sample F e3O4- 0.4@N-C are in 100 mA g-1Cycle performance test chart；
Fig. 6 is sample F e3O4The high rate performance test chart of -0.4@N-C.
Specific implementation mode
The above of the present invention is described in further details by the following examples, but this should not be interpreted as to this The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on the above of the present invention belong to this hair Bright range.
Embodiment
Weigh 0.1 g α-Fe2O3It is added separately to fill 30 mL molar concentrations to be respectively 0.2 mol L-1、0.4 mol L-1、0.6 mol L-1In the beaker of hydrochloric acid solution, 5 min are stirred, mixed solution is transferred in polytetrafluoro reaction kettle in 160 DEG C 12 h of hydro-thermal reaction, centrifuges after being cooled to room temperature, and obtained red precipitate deionized water and ethyl alcohol are distinguished rinse 3 It is secondary, it is dried overnight to obtain the α-Fe of etching processing2O3, it is denoted as α-Fe respectively2O3-0.2、α-Fe2O3-0.4、α-Fe2O3-0.6。
Respectively by 0.3g α-Fe2O3And 0.3 g or more products（α-Fe2O3-0.2、α-Fe2O3-0.4、α-Fe2O3-0.6）Add Enter in the Tris solution for being 10 nM to 150mL molar concentrations, stir 10 min, 0.15 g Dopamine hydrochlorides are added, are stirred under room temperature 6 h are mixed, are washed 3 times with deionized water and ethyl alcohol respectively after solution is centrifuged, are dried overnight to obtain the sample of cladding dopamine, point It is not denoted as α-Fe2O3@PDA、α-Fe2O3-0.2@PDA、α-Fe2O3-0.4@PDA、α-Fe2O3- 0.6@PDA, are dried overnight, in nitrogen Obtained product calcines 4 h in 500 DEG C and obtains Fe under compression ring border3O4@N-C、Fe3O4-0.2@N-C、Fe3O4-0.4@N-C、 Fe3O4-0.6@N-C。
Product will be obtained with PVDF and conductive black according to mass ratio 7:2:1 ratio is coated on copper foil, and thickness is about It is 60 μm, copper foil is cut out to the pole piece for being a diameter of 14 mm with sheet-punching machine, is assembled into 2025 button cells, carries out electrical property survey Examination.
Present invention optimization analyzes in etching process shadow of the different acid concentrations to electrode material high rate performance and cycle performance It rings, by simple hydro-thermal mode to cubical α-Fe2O3Different degrees of etching has been carried out along body-centered direction, has been obtained The cube of porous structure.Then by the carbon coating of N doping and heat treatment, the Fe of carbon coating has been obtained3O4@N-C, to increase The strong structural stability and electric conductivity of electrode material, improves the cycle performance and multiplying power of lithium ion battery to a certain extent Performance.
Fig. 1 is the SEM figures that sample is made in the present embodiment.As shown in Figure 1, the substance and PDF# that are synthesized during experiment α-Fe in 33-06642O3（Hemaite, syn）Diffraction maximum it is consistent, successfully synthesized α-Fe2O3。
Fig. 2 is the SEM figures that sample is made in the present embodiment.As shown in Figure 2, it can be seen that the α-Fe of size uniform2O3By success Synthesis, in N2There is aperture generation after being calcined under environment.According to fig. 2（d-o）, it has been found that after calcining, surface coats sample Dopamine be carbonized and profile becomes coarse and α-Fe2O3It is etched to as porous cube.Meanwhile from Fig. 2（m- o）In it can be seen that, α-Fe2O3Porous structure caved in.
Fig. 3 is the XRD diagram that sample is made in the present embodiment.From figure 3, it can be seen that α-Fe2O3Simultaneously by hydro-thermal etching processing Carry out carbon coating after, during calcining by surface coated dopamine high temperature reduction be Fe3O4（PDF#19-0629）, warp Cross the α-Fe after hydro-thermal etching processing2O3-0.2@PDA、α-Fe2O3- 0.4@PDA and α-Fe2O3- 0.6@PDA are reduced respectively For Fe3O4-0.2@N-C、Fe3O4-0.4@N-C、Fe3O4-0.6@N-C。
Fig. 4 is the TEM figures and Mapping figures that sample is made in embodiment.According to Fig. 4（a）, it can be seen that untreated α- Fe2O3At the cubic of rule, after being etched by hydro-thermal, it may be seen that cubical α-Fe2O3Become porous Structure.After by carbon coating, in Fig. 4（c）In it may be seen that dopamine is not only coated on surface, also edge Body-centered direction cladding.To single Fe3O4-0.4@N-C（Fig. 4（d））Mapping analysis charts（Fig. 4（e-h））, we can be clear Chu sees that Fe, C in sample, N element are evenly distributed.
Fig. 5 is that sample F e is made in the present embodiment3O4- 0.4@N-C are in 100 mA g-1Current density under cycle performance test Figure.Although also there is obvious relaxation phenomenon, capacity has apparent rising after by of short duration decaying, is passing through Specific discharge capacity is maintained at 985.6 mAh g after 200 charge and discharge cycles-1, and specific capacity keeps stabilization not decay.
Fig. 6 is that sample F e is made in the present embodiment3O4High rate performance test charts of -0.4@N-C under different current densities. Fe3O4- 0.4 N-C is passing through the charge and discharge of more powerful ground and is coming back to 100 mA g-1Current density under when, still can Keep 847.6 mAh g-1Reversible capacity.
Embodiment above describes the basic principles and main features and advantage of the present invention, and the technical staff of the industry should Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe the originals of the present invention Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within In the scope of protection of the invention.

Claims (2)

1. a kind of preparation method of nitrogen-doped carbon cladding classification through-hole structure ferroferric oxide composite cathode material, it is characterised in that The specific steps are：
（1）By 0.1 g α-Fe2O3It is 0.2~0.6 mol L to be added to 30 mL molar concentrations-1Hydrochloric acid solution in, stirring 5 Mixed solution is transferred in polytetrafluoro reaction kettle and in 160 DEG C of 12 h of hydro-thermal reaction, is centrifuged after being cooled to room temperature, by institute by min Obtained red precipitate deionized water and ethyl alcohol difference rinse 3 times, the α-of etching processing is obtained then at 60 DEG C of dry 2 h Fe2O3；
（2）By the α-Fe of 0.3 g etching processings2O3It is added in the Tris solution that 150mL molar concentrations are 10 mM, stirring 10 Min is added 0.15 g Dopamine hydrochlorides, stirs 6 h under room temperature, 3 are washed with deionized water and ethyl alcohol respectively after solution is centrifuged It is secondary, the sample of cladding dopamine is obtained then at 60 DEG C of dry 2 h, is then dried overnight, the product that will be obtained in a nitrogen environment 2~4 h are calcined in 500~600 DEG C obtains nitrogen-doped carbon cladding classification through-hole structure ferroferric oxide composite cathode material Fe3O4@ N-C。
2. the preparation of nitrogen-doped carbon cladding classification through-hole structure ferroferric oxide composite cathode material according to claim 1 Method, it is characterised in that：Step（1）Described in the molar concentration of hydrochloric acid solution be preferably 0.4 mol L-1。
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CN108767260A (en) * 2018-06-05 2018-11-06 武汉理工大学 A kind of hollow nano-electrode materials of carbon coating FeP and its preparation method and application
CN110233254A (en) * 2019-07-01 2019-09-13 郑州大学 A kind of lithium ion battery negative material shape Fe that rings a bell3O4/C/MoS2Hydridization particle
CN110813350A (en) * 2019-10-25 2020-02-21 江苏大学 Carbon-based composite electrocatalyst and preparation method and application thereof
CN111117564A (en) * 2019-12-03 2020-05-08 安徽理工大学 Yolk-eggshell type magnetic carbon composite material, preparation method and application
CN111111623A (en) * 2019-12-30 2020-05-08 西安交通大学 Petal-shaped estradiol molecularly imprinted magnetic nano material and preparation method and application thereof
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CN108767260A (en) * 2018-06-05 2018-11-06 武汉理工大学 A kind of hollow nano-electrode materials of carbon coating FeP and its preparation method and application
CN108767260B (en) * 2018-06-05 2021-07-20 武汉理工大学 Carbon-coated FeP hollow nano-electrode material and preparation method and application thereof
KR20200124003A (en) * 2019-04-23 2020-11-02 경희대학교 산학협력단 Anode active material for sodium ion secondary battery and method of preparing the same
KR102214424B1 (en) * 2019-04-23 2021-02-09 경희대학교 산학협력단 Anode active material for sodium ion secondary battery and method of preparing the same
CN110233254A (en) * 2019-07-01 2019-09-13 郑州大学 A kind of lithium ion battery negative material shape Fe that rings a bell3O4/C/MoS2Hydridization particle
CN110233254B (en) * 2019-07-01 2022-05-24 郑州大学 Bell-shaped Fe for lithium ion battery cathode material3O4/C/MoS2Hybrid microparticles
CN110813350A (en) * 2019-10-25 2020-02-21 江苏大学 Carbon-based composite electrocatalyst and preparation method and application thereof
CN110813350B (en) * 2019-10-25 2022-11-18 江苏大学 Carbon-based composite electrocatalyst and preparation method and application thereof
CN111117564A (en) * 2019-12-03 2020-05-08 安徽理工大学 Yolk-eggshell type magnetic carbon composite material, preparation method and application
CN111111623A (en) * 2019-12-30 2020-05-08 西安交通大学 Petal-shaped estradiol molecularly imprinted magnetic nano material and preparation method and application thereof
CN113889610A (en) * 2021-09-26 2022-01-04 山东大学 Method for preparing porous carbon coated transition metal oxide material by CTAB regulation and control and application
CN113889610B (en) * 2021-09-26 2023-06-27 山东大学 Method for preparing porous carbon-coated transition metal oxide material by CTAB regulation and application

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