CN105024053A - Preparation method for carbon nanometer net containing Fe/Fe3C, carbon nanometer net prepared by using same and application of carbon nanometer net - Google Patents

Preparation method for carbon nanometer net containing Fe/Fe3C, carbon nanometer net prepared by using same and application of carbon nanometer net Download PDF

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CN105024053A
CN105024053A CN201510344960.4A CN201510344960A CN105024053A CN 105024053 A CN105024053 A CN 105024053A CN 201510344960 A CN201510344960 A CN 201510344960A CN 105024053 A CN105024053 A CN 105024053A
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carbon nano
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CN105024053B (en
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晏成林
周金秋
钱涛
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Suzhou University
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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
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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Abstract

The invention relates to a preparation method for a carbon nanometer net containing Fe/Fe3C, a carbon nanometer net prepared by using the same and application of the carbon nanometer net. The preparation method comprises the following steps of: (a) adding a pyrrole monomer into water for polymerization reaction to obtain a polypyrrole sphere dispersion liquid; (b) adding a ferrous salt into the dispersion liquid for coordination reaction, and drying the dispersion liquid to obtain a PPy-Fe complex; and (c) placing the PPy-Fe complex in a reducing atmosphere and carrying out calcinations and carbonization. By the preparation method, the Fe/Fe3C is prevented from being directly exposed in an electrolyte so as to protect the stability in the structure and the surface of the Fe/Fe3C, on the other hand, the mechanical stress generated due to the volume expansion of the Fe/Fe3C is relieved better, the polymerization of the Fe/Fe3C is prevented, and structural and electrical integration is kept. Therefore, such electrode material is endowed with high reversible specific capacity and good rate capability, particularly high stability. It is worth noting that the material and the fabrication method can be implemented at a large scale, and high attractiveness is provided for practical application.

Description

Containing Fe/Fe 3the preparation method of the carbon nano net of C, the carbon nano net prepared by the method and application thereof
Technical field
The invention belongs to field of nanometer material technology, relate to a kind of carbon nano net, be specifically related to a kind of containing Fe/Fe 3the preparation method of the carbon nano net of C and the carbon nano net prepared by the method.
Background technology
Nano net structure has a wide range of applications in a lot of field, and this has benefited from its unusual structure and its reconcilable physics and chemical property.The general method of of synthesis of nano web frame uses template.Such as, He et alreport the method utilizing stable NaCl particle as synthetic graphite nano net; Wei et althe control of porosity on the carbon nanosheet utilizing graphene/silicon nanometer sheet template to achieve N doping; Jung et althe film nano hole array having utilized block copolymer as templated synthesis in good order.But, template usually lose time very much and also cost higher, this is because need synthesis template and also experimental procedure a lot.Therefore we are in the urgent need to a kind of easy material carrying out synthesis of nano web frame without template.
Recently, iron shows good performance in field of lithium, such as Fe 3c and derivative thereof, they have many good qualities, and such as theoretical capacity is high, nontoxic, rich content, not perishable, and price is low.But as far as we know, Fe 3c sill is usually used as high performance magnet and catalyst, and in addition, carbide is rarely used in lithium ion battery, and reason has two, and one is volumetric expansion in cyclic process and contraction, and another is that the conductivity of pure carbide is low.In order to solve above stubborn problem, propose a lot of method to promote the structural stability of electrode material.This problem can be able to part by the electrode material of the nanostructure manufacturing different-shape and solve, comprise nano particle, nanometer sheet, nano wire, nanometer rods, nanotube, and hollow nanostructured, because the material of nanostructure is compared with the material of micron dimension, the lithium that can be in harmonious proportion better embeds the tension force in process.Another kind method is material carbonaceous parent being incorporated into synthesis mixing nanostructure in active material.Clearly, the carbon in mixture material has following function: in the material of poorly conductive, promote electric transmission as conductive additive, supports as elastic buffer with the stability promoting electrode.In order to carry out large-scale application, the concept preparing sustainability material by energy-efficient method is very important, such as reproducible organic procedures.A lot of research all manufactures lithium ion battery electrode material by organic procedures.Polypyrrole, as a kind of carbon source of N doping, is that one has good conductivity, energy-storage property, the organic polymer material of redox and capacitive current and calorifics and environmental stability.In addition, a certain amount of N doping can promote the surface wettability degree of material, and capacity and electron conduction keep good cycle performance simultaneously.
Summary of the invention
The present invention seeks to provide a kind of containing Fe/Fe to overcome the deficiencies in the prior art 3the preparation method of the carbon nano net of C.
For achieving the above object, the technical solution used in the present invention is: a kind of containing Fe/Fe 3the preparation method of the carbon nano net of C, it comprises the following steps:
A pyrrole monomer is added to the water and carries out polymerization reaction and obtain polypyrrole ball dispersion liquid by ();
B () adds ferrous salt and carries out complex reaction in described dispersion liquid, obtain PPy-Fe complex after oven dry;
C described PPy-Fe complex is placed in reducing atmosphere and carries out calcining carbonization by ().
Optimally, in step (a), described polymerization reaction is at hydrogen peroxide solution and FeCl 24H 2in 0 ~ 30 DEG C of stirring reaction 3 ~ 8 hours under the initiation of O.
Further, in step (a), pyrrole monomer, hydrogen peroxide solution, FeCl 24H 2the ratio of O and water is 1 ~ 5ml:8 ~ 15ml:0.1 ~ 0.5g:80 ~ 150ml.
Further, in step (a), first in water, add pyrrole monomer, FeCl 24H 2o, drips hydrogen peroxide solution subsequently and carries out polymerization reaction.
Optimally, in step (b), in described dispersion liquid, add FeCl 24H 2o, subsequently drip hydrogen peroxide solution carry out complex reaction within more than 24 hours, make dispersion liquid become clear, dispersion liquid, FeCl 24H 2the ratio of O and hydrogen peroxide solution is 80 ~ 150ml:0.3 ~ 0.5g:15 ~ 25ml.
Further, H in described hydrogen peroxide solution 2o 2mass concentration be 20 ~ 35%.
Optimally, in step (c), described reducing atmosphere is argon gas and hydrogen composition, and its volume flow ratio is 3 ~ 8:1, and calcining heat is 600 ~ 1100 DEG C.
Another object of the present invention be to provide a kind of said method to prepare containing Fe/Fe 3the carbon nano net of C.
Another object of the present invention is to provide a kind of containing Fe/Fe 3the application of carbon nano net in lithium ion battery negative material of C.
Because technique scheme is used, the present invention compared with prior art has following advantages: the present invention is containing Fe/Fe 3the preparation method of the carbon nano net of C, employs a kind of easy method without template and has synthesized and include Fe/Fe 3the carbon nanometer mesh material of the N doping of C (is called for short N-Fe/Fe 3c@C), make Fe/Fe 3c is coated by carbon nanomaterial, avoids Fe/Fe 3c is directly exposed in electrolyte and protects Fe/Fe 3the structure of C and surface stability, be also in harmonious proportion by Fe/Fe on the other hand well 3c volumetric expansion and the mechanical tension produced, inhibit Fe/Fe 3the polymerization of C, therefore maintains structure and electrical integrity.Therefore, this electrode material shows very high reversible specific capacity, and high rate performance is all well and good, and particularly stability is fine.It should be noted that material and manufacture method all can be prepared on a large scale, very attractive for practical application.
Accompanying drawing explanation
Accompanying drawing 1 is for the present invention is containing Fe/Fe 3the state change map of mixed liquor in the preparation method of the carbon nano net of C;
Accompanying drawing 2 is for the present invention is containing Fe/Fe 3the step schematic diagram of the carbon nano net preparation method of C;
Accompanying drawing 3 is N-Fe/Fe prepared by the embodiment of the present invention 1 3the scanning electron microscope (SEM) photograph of C@C;
Accompanying drawing 4 is the scanning electron microscope (SEM) photograph of N-Fe/Fe3C@C prepared by the embodiment of the present invention 2;
Fig. 5 is N-Fe/Fe prepared by the embodiment of the present invention 2 3the multiplying power of C@C and cycle performance figure.
Embodiment
The present invention is containing Fe/Fe 3the preparation method of the carbon nano net of C, it comprises the following steps: pyrrole monomer is added to the water and carries out polymerization reaction and obtain polypyrrole ball dispersion liquid by (a); B () adds ferrous salt and carries out complex reaction in described dispersion liquid, obtain PPy-Fe complex after oven dry; C described PPy-Fe complex is placed in reducing atmosphere and carries out calcining carbonization by (), as shown in Figure 2.Employ a kind of easy method without template to have synthesized and include Fe/Fe 3the carbon nanometer mesh material of the N doping of C (is called for short N-Fe/Fe 3c@C), make Fe/Fe 3c is coated by carbon nanomaterial, avoids Fe/Fe 3c is directly exposed in electrolyte and protects Fe/Fe 3the structure of C and surface stability, be also in harmonious proportion by Fe/Fe on the other hand well 3c volumetric expansion and the mechanical tension produced, inhibit Fe/Fe 3the polymerization of C, therefore maintains structure and electrical integrity.Therefore, this electrode material shows very high reversible specific capacity, and high rate performance is all well and good, and particularly stability is fine.It should be noted that material and manufacture method all can be prepared on a large scale, very attractive for practical application.
In step (a), described polymerization reaction is at hydrogen peroxide solution and FeCl 24H 2in 0 ~ 30 DEG C of stirring reaction 3 ~ 8 hours under the initiation of O.Pyrrole monomer, hydrogen peroxide solution, FeCl 24H 2the ratio of O and water is 1 ~ 5ml:8 ~ 15ml:0.1 ~ 0.5g:80 ~ 150ml.In step (a), first in water, add pyrrole monomer, FeCl 24H 2o, drips hydrogen peroxide solution subsequently and carries out polymerization reaction.
In step (b), in described dispersion liquid, add FeCl 24H 2o, subsequently drip hydrogen peroxide solution carry out complex reaction within more than 24 hours, make dispersion liquid become clear as shown in Figure 1, dispersion liquid, FeCl 24H 2the ratio of O and hydrogen peroxide solution is 80 ~ 150ml:0.3 ~ 0.5g:15 ~ 25ml.H in described hydrogen peroxide solution 2o 2mass concentration be 20 ~ 35%.
In step (c), described reducing atmosphere is argon gas and hydrogen composition, and its volume flow ratio is 3 ~ 8:1, and calcining heat is 600 ~ 1100 DEG C.
N-Fe/Fe will be obtained 3c@C, acetylene black, PTFE binding agent mix with the mass ratio of 7:2:1, are coated in nickel foam and make electrode, electrode slice at 60 DEG C vacuumize 24h as negative pole; With lithium sheet as to electrode, the LiPF of 1 mol/L 6be dissolved in ethylene carbonate (EC), methyl ethyl ester (EMC), diethyl carbonate (DEC) by volume in the electrolyte that is mixed to form of 4:3:3 as electrolyte, Celgard 2400 is made into button cell (CR2025) as barrier film.
Below in conjunction with accompanying drawing embodiment, the present invention is further described.
Embodiment 1
The present embodiment provides a kind of and uses PPy-Fe complex preparation N-Fe/Fe 3c@C nano mesh material, as the method for lithium ion battery negative material, is specially:
A (), under room temperature environment, adds the H of 88 mL in three-neck flask 2o, 2 mL pyrroles, 0.2 g FeCl 24H 2o, then slowly drips 10 mL H 2o 2, stir 6 h;
B () adds 0.6 g FeCl 24H 2o, then slowly drips 30 mL H 2o 2; Stir 24 more than h, solution becomes clear gradually, in glassy yellow;
C () is by described PPy-Fe complex vacuum drying;
(d) in tube furnace at Ar (200 sccm) and H 2under the atmosphere of (40 sccm), 900 oC calcine 2 h;
E () is by described N-Fe/Fe 3c@C nano mesh material makes lithium ion battery negative material; Its scanning electron microscope (SEM) photograph as shown in Figure 3.
Embodiment 2
The present embodiment provides a kind of and uses PPy-Fe complex preparation N-Fe/Fe 3c@C nano mesh material as the method for lithium ion battery negative material, substantially identical with embodiment 1 of its concrete steps, different unlike reagent quality, be specially:
A (), under room temperature environment, adds the H of 88 mL in three-neck flask 2o, 2 mL pyrroles, 0.2 g FeCl 24H 2o, then slowly drips 10 mL H 2o 2.Stir 6 h;
B () adds 0.34 g FeCl 24H 2o, then slowly drips 17 mL H 2o 2.Stir 24 more than h, solution becomes clear gradually, in glassy yellow;
C () is by described PPy-Fe complex vacuum drying;
(d) in tube furnace at Ar (200 sccm) and H 2under the atmosphere of (40 sccm), 900 oC calcine 2 h;
E () is by described N-Fe/Fe 3c@C nano mesh material makes lithium ion battery negative material, and as shown in Figure 3, its high rate performance and cycle performance are as shown in Figure 4 for its scanning electron microscope (SEM) photograph.
Embodiment 3
The present embodiment provides a kind of and uses PPy-Fe complex preparation N-Fe/Fe 3c@C nano mesh material as the method for lithium ion battery negative material, substantially identical with embodiment 1 of its concrete steps, different unlike reagent quality, be specially:
A (), at 0 DEG C, adds the H of 80 mL in three-neck flask 2o, 1 mL pyrroles, 0.1 g FeCl 24H 2o, then slowly drips (1 drop/sec) 8 mL H 2o 2(20wt%), 3h is stirred;
B () adds 0.3g FeCl 24H 2o, then slowly drips 15 mL H 2o 2; Stir 24 more than h, solution becomes clear gradually, in glassy yellow;
C () is by described PPy-Fe complex vacuum drying;
(d) in tube furnace at Ar (120 sccm) and H 2lower 600 DEG C of calcining 5 h of atmosphere of (40 sccm).
Embodiment 4
The present embodiment provides a kind of and uses PPy-Fe complex preparation N-Fe/Fe 3c@C nano mesh material as the method for lithium ion battery negative material, substantially identical with embodiment 1 of its concrete steps, different unlike reagent quality, be specially:
A (), at 30 DEG C, adds the H of 150 mL in three-neck flask 2o, 5mL pyrroles, 0.5g FeCl 24H 2o, then slowly drips (2 drops/sec) 15mL H 2o 2(35wt%); Stir 8h;
B () adds 0.5 g FeCl 24H 2o, then slowly drips 25mL H 2o 2.Stir 24 more than h, solution becomes clear gradually, in glassy yellow;
C () is by described PPy-Fe complex vacuum drying;
(d) in tube furnace at Ar (320 sccm) and H 2the lower 1100 DEG C of calcining 1h of atmosphere of (40 sccm);
Above-described embodiment is only for illustrating technical conceive of the present invention and feature; its object is to person skilled in the art can be understood content of the present invention and implement according to this; can not limit the scope of the invention with this; all equivalences done according to Spirit Essence of the present invention change or modify, and all should be encompassed within protection scope of the present invention.

Claims (9)

1. one kind contains Fe/Fe 3the preparation method of the carbon nano net of C, it is characterized in that, it comprises the following steps:
A pyrrole monomer is added to the water and carries out polymerization reaction and obtain polypyrrole ball dispersion liquid by ();
B () adds ferrous salt and carries out complex reaction in described dispersion liquid, obtain PPy-Fe complex after oven dry;
C described PPy-Fe complex is placed in reducing atmosphere and carries out calcining carbonization by ().
2. according to claim 1 containing Fe/Fe 3the preparation method of the carbon nano net of C, is characterized in that: in step (a), and described polymerization reaction is at hydrogen peroxide solution and FeCl 24H 2in 0 ~ 30 DEG C of stirring reaction 3 ~ 8 hours under the initiation of O.
3. according to claim 2 containing Fe/Fe 3the preparation method of the carbon nano net of C, is characterized in that: in step (a), pyrrole monomer, hydrogen peroxide solution, FeCl 24H 2the ratio of O and water is 1 ~ 5ml:8 ~ 15ml:0.1 ~ 0.5g:80 ~ 150ml.
4. according to claim 3 containing Fe/Fe 3the preparation method of the carbon nano net of C, is characterized in that: in step (a), first in water, adds pyrrole monomer, FeCl 24H 2o, drips hydrogen peroxide solution subsequently and carries out polymerization reaction.
5. according to claim 1 containing Fe/Fe 3the preparation method of the carbon nano net of C, is characterized in that: in step (b), in described dispersion liquid, add FeCl 24H 2o, subsequently drip hydrogen peroxide solution carry out complex reaction within more than 24 hours, make dispersion liquid become clear, dispersion liquid, FeCl 24H 2the ratio of O and hydrogen peroxide solution is 80 ~ 150ml:0.3 ~ 0.5g:15 ~ 25ml.
6. according to claim 2 or 4, contain Fe/Fe 3the preparation method of the carbon nano net of C, is characterized in that: H in described hydrogen peroxide solution 2o 2mass concentration be 20 ~ 35%.
7. according to claim 1 containing Fe/Fe 3the preparation method of the carbon nano net of C, is characterized in that: in step (c), and described reducing atmosphere is argon gas and hydrogen composition, and its volume flow ratio is 3 ~ 8:1, and calcining heat is 600 ~ 1100 DEG C.
8. one kind contains Fe/Fe 3the carbon nano net of C, is prepared from by described preparation method arbitrary in claim 1 to 7.
9. contain Fe/Fe described in claim 8 3the application of carbon nano net in lithium ion battery negative material of C.
CN201510344960.4A 2015-06-19 2015-06-19 Contain Fe/Fe3The preparation method of the carbon nano net of C, the carbon nano net prepared with the method and its application Active CN105024053B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106067546A (en) * 2016-08-10 2016-11-02 上海交通大学 Carbon/nano silicon carbide two iron composite material, combination electrode and preparation method and application
CN106532021A (en) * 2017-01-11 2017-03-22 安徽工业大学 Fe<3>C@onion-shaped carbon/amorphous carbon nanocomposite and preparation method and application thereof
CN110289403A (en) * 2019-06-12 2019-09-27 苏州大学 A kind of Nano carbon balls and its preparation method and application containing monatomic Fe

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CN104393313A (en) * 2014-12-04 2015-03-04 黑龙江大学 Nitrogen-doped Fe/Fe3C/C microbial fuel cell cathode catalyst material and preparation method thereof

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CN104393313A (en) * 2014-12-04 2015-03-04 黑龙江大学 Nitrogen-doped Fe/Fe3C/C microbial fuel cell cathode catalyst material and preparation method thereof

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LIWEI SU ET AL: "Core-shell Fe@Fe3C/C nanocomposites as anode materials for Li ion batteries", 《ELECTROCHIMICA ACTA》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106067546A (en) * 2016-08-10 2016-11-02 上海交通大学 Carbon/nano silicon carbide two iron composite material, combination electrode and preparation method and application
CN106532021A (en) * 2017-01-11 2017-03-22 安徽工业大学 Fe<3>C@onion-shaped carbon/amorphous carbon nanocomposite and preparation method and application thereof
CN110289403A (en) * 2019-06-12 2019-09-27 苏州大学 A kind of Nano carbon balls and its preparation method and application containing monatomic Fe

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