CN105514374A - Graphitized carbon coated manganese-fluorine oxide material and preparation method thereof - Google Patents

Graphitized carbon coated manganese-fluorine oxide material and preparation method thereof Download PDF

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CN105514374A
CN105514374A CN201510919439.9A CN201510919439A CN105514374A CN 105514374 A CN105514374 A CN 105514374A CN 201510919439 A CN201510919439 A CN 201510919439A CN 105514374 A CN105514374 A CN 105514374A
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manganese
preparation
graphitized carbon
solution
oxide material
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CN105514374B (en
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唐浩林
魏希
王锐
蔡世昌
曾燕
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Wuhan University of Technology WUT
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • 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
    • H01M4/582—Halogenides
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a graphitized carbon coated manganese-fluorine oxide material, prepared by mixing manganese source and perfluorinated sulfonic acid resin solution and carbonizing the mixture. A preparation method of the graphitized carbon coated manganese-fluorine oxide material comprises the concrete steps of mixing the manganese source solution and perfluorinated sulfonic acid resin, and evenly stirring; then, adjusting a pH of the mixed solution; after a stirring reaction, sequentially drying and carrying out roasting carbonization to obtain the graphitized carbon coated manganese-fluorine oxide material. The carbon in the graphitized carbon coated manganese-fluorine oxide material is in a graphitized state, so that an ion and electron transport rate of the material can be greatly improved; the graphitized carbon coated manganese-fluorine oxide material can be taken as a high cycle stability lithium ion battery cathode material; furthermore, the preparation technology is simple and short in synthesizing time, thus being suitable for popularization and application.

Description

Coated manganese OXYFLUORIDE MATERIALS of a kind of graphitized carbon and preparation method thereof
Technical field
The invention belongs to new energy materials field, be specifically related to coated manganese OXYFLUORIDE MATERIALS of a kind of graphitized carbon and preparation method thereof.
Background technology
Lithium ion battery (LiBs) is widely used in the portable communication apparatus such as mobile phone, notebook computer due to advantages such as voltage are high, capacity large, have extended cycle life.But lithium ion battery negative material commercial is at present based on graphite material, the theoretical capacity of graphite only has 372mAh/g, cannot meet high-capacity lithium ion cell needs of new generation.The material with carbon element (as carbon nano-tube, mesoporous carbon) novel compared to graphite material and transition group metallic oxide (as manganese oxide, iron oxide, nickel oxide, cupric oxide etc.) have higher specific capacity.But the great variety of metal oxide inevitably along with volume in charge and discharge process, cause the efflorescence of electrode material, thus cause the rapid decay of capacity.
In numerous transition metal oxide, the voltage delay of MnO is relatively little (<0.8V), the higher (5.43g/cm of density 3), and there is specific capacity high (theoretical value 755.6mAh/g) and the low (1.032V (vsLi/Li of electromotive force +)) etc. feature, be the very potential lithium ion battery negative material of one.But the same with other transition metal oxide, in low conductivity and charge and discharge process, large change in volume has had a strong impact on the capacity of this material, multiplying power and cycle performance, constrains its fast development in field of lithium ion battery and application.
Researchers once adopted and controlled particle size, and prepare micro nano structure, pore structure, sheet MnO negative material, the methods such as material with carbon-coated surface improve the chemical property of Mn oxide.Such as, MnO film prepared by Li Hong research group, MnO/C composite material and MnO/C multi-pore micron ball improve the battery performance of MnO material all to a certain extent, and wherein MnO/C composite material shows the reversible capacity of 400mAh/g under the electric current of 400mA/g.The MnO/C Coaxial Nanotubes of the preparation such as Ding can discharge reversible specific capacity (the fourth friend of 600mAh/g under the current density of 75.5mA/g, Xu Youlong, Sun Xiaofei. fabrication & properties [J] .ActaPhys.Chim.Sin of nanometer MnO lithium ion battery negative material, 2013,29:1.).The nucleocapsid structure MnO/C nanometer rods of the preparation such as nano-sheet MnO negative material and Sun also improves the chemical property of MnO to a certain extent.But the technical process of these modified measures is all comparatively complicated, and manufacturing cost is higher, the more important thing is and promotes limited to the chemical property of MnO, and distance industrialization practical application is still far away.
Summary of the invention
The object of this invention is to provide a kind of graphitized carbon coated manganese oxygen fluoride material and preparation method thereof, graphitized carbon material is adopted to be undertaken coated by metal oxyfluoride, the advantage of and graphitized carbon material good conductivity high in conjunction with oxide capacity, avoid the structural defect of homogenous material, the problem such as prevent electrode material change in volume excessive, improves its cyclical stability; And the preparation technology related to is simple, generated time is short, is applicable to applying.
For achieving the above object, the technical solution used in the present invention is:
A preparation method for the coated manganese OXYFLUORIDE MATERIALS of graphitized carbon, is characterized in that, comprise the following steps:
1) by soluble in water for manganese source, stir to obtain manganese source solution for standby; Prepare uniform alkaline solution of sodium hydroxide for subsequent use;
2) mixed with perfluor sulfoacid resin solution by manganese source solution, stir to obtain mixed liquor I;
3) regulate the pH value of mixed liquor I by alkaline solution of sodium hydroxide, stirring reaction 4 ~ 8h, obtains mixed liquor I I, then mixed liquor I I is carried out drying;
4) by step 3) gained desciccate carries out roasting charing, obtains the coated manganese OXYFLUORIDE MATERIALS of described graphitized carbon.
In such scheme, described alkaline solution of sodium hydroxide is sodium hydrate aqueous solution, NaOH aqueous isopropanol or NaOH ethanolic solution.
In such scheme, described manganese source is manganese nitrate, manganese sulfate or manganese acetate.
In such scheme, the addition of described manganese source and perfluor sulfoacid resin solution is as the criterion with the Mn provided and C element respectively, and wherein the mass ratio of Mn element and C element is 8:1 ~ 1:16.
In such scheme, step 3) described pH value is 6 ~ 8.
In such scheme, described 3) described baking temperature is 50 ~ 80 DEG C, and drying time is 8 ~ 12h.
In such scheme, described roasting carbonization temperature is 600 ~ 900 DEG C, and heating rate is 0.5 ~ 10 DEG C/min, and temperature retention time is 1 ~ 6h.
In such scheme, the atmosphere that described roasting carbonization adopts is argon gas or nitrogen.
According to the coated manganese OXYFLUORIDE MATERIALS of graphitized carbon prepared by such scheme, it is formed by graphitized carbon coated manganese oxyfluoride nano particle, can be used as lithium cell cathode material.
The precursor power graphitized carbon coated manganese oxygen fluoride material that the present invention adopts liquid phase synthesizing method directly to obtain, and adopt the method for electrostatic self-assembled, sulfonate radical is made to wrap up manganese ion, and carry out carbonization, realize the coated process of graphitized carbon at manganese oxygen fluoride nano grain surface, construct and be uniformly dispersed and there is the material of excellent electrochemical performance, can be used as a kind of lithium cell cathode material of electrochemical performance.
Compared with prior art, the invention has the beneficial effects as follows:
1), in the coated manganese OXYFLUORIDE MATERIALS of graphitized carbon of the present invention, the carbon of coated manganese oxygen fluoride material is graphitization state, greatly improves ion and the electron transfer rate of material; And manganese oxygen fluoride is Nanoparticulate, size tunable.
2) coated for graphitized carbon of the present invention manganese oxygen fluoride material is used as lithium ion battery negative material, its cyclical stability is excellent, and also has broad application prospects as electrode material for super capacitor.
3) preparation method that the present invention relates to is simple, and the cycle is short, and experiment condition is simple, is applicable to applying.
Accompanying drawing explanation
Fig. 1 is that the transmission electron microscope TEM of gained mixed liquor I I in the embodiment of the present invention 1 schemes.
Fig. 2 is that the transmission electron microscope TEM of roasting carbonization products therefrom in the embodiment of the present invention 1 schemes.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but the present invention is not only confined to the following examples.
Following examples as no specific instructions, the commercially available chemical reagent of reagent of employing or industrial products.
Embodiment 1
A kind of graphitized carbon coated manganese oxygen fluoride material, its preparation method comprises the following steps:
1) prepare saturated NaOH aqueous isopropanol, stir stand-by; Get 60ml perfluor sulfoacid resin solution and be placed in there-necked flask, magnetic agitation is even; Mn and the C mass ratio provided according to manganese source and perfluor sulfoacid resin solution is that the ratio of 1:16 takes manganese acetate, adds in 10ml deionized water, magnetic agitation uniform dissolution, obtains uniform manganese acetate solution;
2) in perfluor sulfoacid resin solution, slowly drip manganese acetate solution, mix and blend 1h, obtains mixed liquor I;
3) in mixed solution I, slowly drip the NaOH aqueous isopropanol prepared, regulate its pH to be 7, magnetic agitation reaction 8h obtains mixed liquor I I, mixed liquor I I is placed in 50 DEG C of dry 12h of air dry oven.
4) dried product exhibited is put into aluminium oxide porcelain boat, and be placed in tube furnace, first at room temperature with the high-purity Ar gas flow purging 2h of 100mL/min, then air-flow is decreased to 60mL/min, carry out roasting carbonization with the ramp to 800 of 5 DEG C/min DEG C, insulation 90min, cools to room temperature with the furnace, obtain black powder, be the coated manganese OXYFLUORIDE MATERIALS of described graphitized carbon.
The transmission electron microscope TEM figure of the present embodiment gained mixed liquor I I is shown in Fig. 1; The transmission electron microscope TEM figure of roasting products therefrom is shown in Fig. 2.From Fig. 1,2, the even particle distribution of gained manganese oxyfluoride, its surface coated carbon is graphitization state.Be applied to by coated for the graphitized carbon of preparation manganese OXYFLUORIDE MATERIALS and prepare lithium ion battery negative, it is at 50mAg -1current density under circulation 60 circle after discharge capacity be 347mAhg -1, at 200mAg -1current density under circulation 200 circle after discharge capacity be 312mAhg -1, there is excellent cyclical stability.
Embodiment 2
A kind of graphitized carbon coated manganese oxygen fluoride material, its preparation method comprises the following steps:
1) prepare saturated NaOH aqueous isopropanol, stir stand-by; Get 60ml perfluor sulfoacid resin solution and be placed in there-necked flask, magnetic agitation is even; Mn and the C mass ratio provided according to manganese source and perfluor sulfoacid resin solution is that the ratio of 8:1 takes manganese acetate, adds in 10ml deionized water, magnetic agitation uniform dissolution, obtains uniform manganese acetate solution;
2) in perfluor sulfoacid resin solution, slowly drip manganese acetate solution, mix and blend 1h, obtains mixed liquor I;
3) in mixed solution I, slowly drip the NaOH aqueous isopropanol prepared, regulate its pH to be 6, magnetic agitation reaction 4h, obtains mixed liquor I I, mixed liquor I I is placed in 50 DEG C of dry 12h of air dry oven.
4) dried product exhibited is put into aluminium oxide porcelain boat, and be placed in tube furnace, first at room temperature with the high-purity Ar gas flow purging 2h of 100mL/min, then air-flow is decreased to 60mL/min, carry out roasting carbonization with the ramp to 600 of 1 DEG C/min DEG C, insulation 60min, cools to room temperature with the furnace, obtain black powder, the i.e. coated manganese OXYFLUORIDE MATERIALS of graphitized carbon.
The coated manganese OXYFLUORIDE MATERIALS of the graphitized carbon prepared by the present embodiment is applied to prepares lithium ion battery negative, and it is at 50mAg -1current density under circulation 60 circle after discharge capacity be 645mAhg -1, at 200mAg -1current density under circulation 200 circle after discharge capacity be 721mAhg -1, there is excellent cyclical stability.
Embodiment 3
A kind of graphitized carbon coated manganese oxygen fluoride material, its preparation method comprises the following steps:
1) prepare saturated NaOH aqueous isopropanol, stir stand-by; Get 60ml perfluor sulfoacid resin solution and be placed in there-necked flask, magnetic agitation is even; Mn and the C mass ratio provided according to manganese source and perfluor sulfoacid resin solution is that the ratio of 8:1 takes manganese sulfate, adds in 10ml deionized water, magnetic agitation uniform dissolution, obtains uniform manganese sulfate solution;
2) in perfluor sulfoacid resin solution, slowly drip manganese sulfate solution, mix and blend 1h, obtains mixed liquor I;
3) in mixed solution I, slowly drip the NaOH aqueous isopropanol prepared, regulate its pH to be 8, magnetic agitation reaction 8h, obtains mixed liquor I I, mixed liquor I I is placed in 80 DEG C of dry 8h of air dry oven.
4) dried product exhibited is put into aluminium oxide porcelain boat, and be placed in tube furnace, first at room temperature with the high-purity Ar gas flow purging 2h of 100mL/min, then air-flow is decreased to 60mL/min, carry out roasting carbonization with the ramp to 800 of 5 DEG C/min DEG C, insulation 90min, cools to room temperature with the furnace, obtain black powder, the i.e. coated manganese OXYFLUORIDE MATERIALS of graphitized carbon.
The coated manganese OXYFLUORIDE MATERIALS of the graphitized carbon prepared by the present embodiment is applied to prepares lithium ion battery negative, and it is at 50mAg -1current density under circulation 60 circle after discharge capacity be 535mAhg -1, at 200mAg -1current density under circulation 200 circle after discharge capacity be 425mAhg -1, there is excellent cyclical stability.
Embodiment 4
A kind of graphitized carbon coated manganese oxygen fluoride material, its preparation method comprises the following steps:
1) prepare saturated NaOH aqueous isopropanol, stir stand-by; Get 60ml perfluor sulfoacid resin solution and be placed in there-necked flask, magnetic agitation is even; Mn and the C mass ratio provided according to manganese source and perfluor sulfoacid resin solution is that the ratio of 4:1 takes manganese sulfate, adds in 10ml deionized water, magnetic agitation uniform dissolution, obtains uniform manganese sulfate solution;
2) in perfluor sulfoacid resin solution, slowly drip manganese sulfate solution, mix and blend 1h, obtains mixed liquor I;
3) in mixed solution I, slowly drip the NaOH aqueous isopropanol prepared, regulate its pH to be 7, magnetic agitation reaction 8h, obtains mixed liquor I I, mixed liquor I I is placed in 60 DEG C of dry 10h of air dry oven;
4) dried product exhibited is put into aluminium oxide porcelain boat, and be placed in tube furnace, first at room temperature with the high-purity Ar gas flow purging 2h of 100mL/min, then air-flow is decreased to 60mL/min, carry out roasting carbonization with the ramp to 900 of 10 DEG C/min DEG C, insulation 6h, cools to room temperature with the furnace, obtain black powder, the i.e. coated manganese OXYFLUORIDE MATERIALS of graphitized carbon.
The coated manganese OXYFLUORIDE MATERIALS of the graphitized carbon prepared by the present embodiment is applied to prepares lithium ion battery negative, and it is at 50mAg -1current density under circulation 60 circle after discharge capacity be 417mAhg -1, at 200mAg -1current density under circulation 200 circle after discharge capacity be 521mAhg -1, there is excellent cyclical stability.
Each pulp furnish cited by the present invention can realize the present invention, and the bound value of each raw material, interval value can realize the present invention, and the bound value of technological parameter of the present invention and interval value can realize the present invention, do not enumerate embodiment at this.

Claims (9)

1. a preparation method for the coated manganese OXYFLUORIDE MATERIALS of graphitized carbon, is characterized in that, comprise the following steps:
1) by soluble in water for manganese source, stir to obtain manganese source solution for standby; Prepare uniform alkaline solution of sodium hydroxide for subsequent use;
2) mixed with perfluor sulfoacid resin solution by manganese source solution, stir to obtain mixed liquor I;
3) regulate the pH value of mixed liquor I by alkaline solution of sodium hydroxide, stirring reaction 4 ~ 8h, obtains mixed liquor I I, then mixed liquor I I is carried out drying;
4) by step 3) gained desciccate carries out roasting charing, obtains the coated manganese OXYFLUORIDE MATERIALS of described graphitized carbon.
2. preparation method according to claim 1, is characterized in that, described alkaline solution of sodium hydroxide is sodium hydrate aqueous solution, NaOH aqueous isopropanol or NaOH ethanolic solution.
3. preparation method according to claim 1, is characterized in that, described manganese source is manganese nitrate, manganese sulfate or manganese acetate.
4. preparation method according to claim 1, is characterized in that, the addition of described manganese source and perfluor sulfoacid resin solution is as the criterion with the Mn provided and C element respectively, and wherein the mass ratio of Mn element and C element is 8:1 ~ 1:16.
5. preparation method according to claim 1, is characterized in that, step 3) described pH value is 6 ~ 8.
6. preparation method according to claim 1, is characterized in that, described 3) described baking temperature is 50 ~ 80 DEG C, and drying time is 8 ~ 12h.
7. preparation method according to claim 1, is characterized in that, described roasting carbonization temperature is 600 ~ 900 DEG C, and heating rate is 0.5 ~ 10 DEG C/min, and temperature retention time is 1 ~ 6h.
8. preparation method according to claim 1, is characterized in that, the atmosphere that described roasting carbonization adopts is argon gas or nitrogen.
9. the coated manganese OXYFLUORIDE MATERIALS of the graphitized carbon that described in any one of claim 1 ~ 8 prepared by preparation method, is characterized in that, it is formed by graphitized carbon coated manganese oxyfluoride nano particle.
CN201510919439.9A 2015-12-11 2015-12-11 A kind of graphitized carbon cladding manganese OXYFLUORIDE MATERIALS and preparation method thereof Expired - Fee Related CN105514374B (en)

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Publication number Priority date Publication date Assignee Title
CN110828784A (en) * 2018-08-13 2020-02-21 比亚迪股份有限公司 Lithium battery positive electrode material and preparation method and application thereof
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CN112436128A (en) * 2020-12-01 2021-03-02 上海纳米技术及应用国家工程研究中心有限公司 Preparation method of manganese-cobalt-oxygen composite two-dimensional carbon material for lithium ion battery cathode
CN113224302A (en) * 2021-05-08 2021-08-06 陕西科技大学 Iron cyanamide material for realizing graphitized carbon coating by in-situ autocatalysis and application thereof

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