CN105024053B - Contain Fe/Fe3The preparation method of the carbon nano net of C, the carbon nano net prepared with the method and its application - Google Patents
Contain Fe/Fe3The preparation method of the carbon nano net of C, the carbon nano net prepared with the method and its application Download PDFInfo
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Abstract
The present invention relates to a kind of contain Fe/Fe3The preparation method of the carbon nano net of C, the carbon nano net prepared with the method and its application, it comprises the following steps：（a）Pyrrole monomer is added to the water to carry out polyreaction and obtains polypyrrole ball dispersion liquid；（b）To in the dispersion liquid, add ferrous salt to carry out complex reaction, after drying, obtain PPy Fe coordination compounds；（c）The PPy Fe coordination compounds are placed in reducing atmosphere carries out calcining carbonization.Avoid Fe/Fe3C is directly exposed in electrolyte and protects Fe/Fe3The structure and surface stability of C, has on the other hand also well reconciled by Fe/Fe3C volumetric expansions and the mechanical tension that produces, it is suppressed that Fe/Fe3The 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, for practical application very attractive.
Description
Technical field
The invention belongs to field of nanometer material technology, is related to a kind of carbon nano net, and in particular to a kind of containing Fe/Fe3The carbon nanometer of C
The preparation method of net and the carbon nano net prepared with the method.
Background technology
Nanometer web frame have a wide range of applications in a lot of fields, this have benefited from its unusual construction and its adjustable and
Physics and chemical property.One universal method of synthesis nanometer web frame is to use template.Such as, Heet alReport
By the use of stable NaCl granules as the method for synthetic graphite nano net；Weiet alUsing graphene/silicon nanometer sheet template
Achieve the control of porosity on the carbon nanosheet to N doping；Junget alBy the use of block copolymer as templated synthesis
Film nano hole array in good order.But, template is generally lost time and relatively costly very much, this is because needing to close
Into template and experimental procedure is a lot.Therefore we synthesize the material of nanometer web frame in the urgent need to a kind of easy template-free method
Material.
Recently, iron shows good performance in field of lithium, such as Fe3C and its derivant, they have
Lot of advantages, such as theoretical capacity are high, nontoxic, rich content, and not perishable, price is low.But as far as we know, Fe3C bases
Material is usually as high performance magnet and catalyst, in addition, carbide is rarely used in lithium ion battery, reason has two, and one
Individual is volumetric expansion and contraction in cyclic process, another be pure carbide electric conductivity low.Above thorny in order to solve
Problem, it is proposed that a lot of methods are lifting the structural stability of electrode material.This problem can pass through to manufacture different-shape
The electrode material of nanostructured be able to part solution, including nano-particle, nanometer sheet, nano wire, nanometer rods, nanotube, with
And hollow nanostructured, because the material of nanostructured is compared with the material of micron dimension, the embedded abjection of the lithium that preferably can reconcile
During tension force.Another kind of method is the material for carbonaceous parent being incorporated into synthesis mixing nanostructured in active material.Very
Substantially, the carbon in mixture material has following function：Electronics is lifted as conductive additive in the material of poorly conductive
Transmission, supports to lift the stability of electrode as elastic buffer.In order to be able to carry out large-scale application, with energy-efficient method
The concept for preparing sustainability material is critically important, such as reproducible organic procedures.A lot of researchs all pass through organic procedures system
Make lithium ion battery electrode material.Polypyrrole, as a kind of carbon source of N doping, is that one kind has good electric conductivity, energy storage
Performance, oxidoreduction and capacitive current and the organic polymer material of calorifics and environmental stability.In addition, a certain amount of nitrogen
Doping can lift the surface wettability degree of material, capacity and electron conduction, while keeping good cycle performance.
Content of the invention
The invention aims to overcoming the deficiencies in the prior art and providing a kind of containing Fe/Fe3The preparation of the carbon nano net of C
Method.
For reaching above-mentioned purpose, the technical solution used in the present invention is：One kind contains Fe/Fe3The preparation side of the carbon nano net of C
Method, it are comprised the following steps：
（a）Pyrrole monomer is added to the water to carry out polyreaction and obtains polypyrrole ball dispersion liquid；
（b）To in the dispersion liquid, add ferrous salt to carry out complex reaction, after drying, obtain PPy-Fe coordination compounds；
（c）The PPy-Fe coordination compounds are placed in reducing atmosphere carries out calcining carbonization.
Optimally, step（a）In, the polyreaction is in hydrogen peroxide solution and FeCl2·4H2In 0 ~ 30 under the initiation of O
DEG C stirring reaction 3 ~ 8 hours.
Further, step（a）In, pyrrole monomer, hydrogen peroxide solution, FeCl2·4H2The ratio of O and water is 1 ~ 5ml：8~
15ml：0.1~0.5g：80~150ml.
Further, step（a）In, in water, first add pyrrole monomer, FeCl2·4H2O, subsequent Deca hydrogen peroxide solution
Carry out polyreaction.
Optimally, step（b）In, FeCl is added in the dispersion liquid2·4H2O, subsequent Deca hydrogen peroxide solution are carried out
Complex reaction makes dispersion liquid become clear, dispersion liquid, FeCl for more than 24 hours2·4H2The ratio of O and hydrogen peroxide solution be 80 ~
150ml：0.3~0.5g：15~25ml.
Further, H in the hydrogen peroxide solution2O2Mass concentration be 20 ~ 35%.
Optimally, step（c）In, the reducing atmosphere is that argon and hydrogen are constituted, and its volume flow ratio is 3 ~ 8：1,
Calcining heat is 600 ~ 1100 DEG C.
A further object of the present invention is to provide that prepared by a kind of said method containing Fe/Fe3The carbon nano net of C.
It is still another object of the present invention to provide a kind of contain Fe/Fe3The carbon nano net of C is in lithium ion battery negative material
Application.
As above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：The present invention contains Fe/Fe3C
Carbon nano net preparation method, used a kind of easy method without template to synthesize and included Fe/Fe3The N doping of C
Carbon nanometer mesh material（Abbreviation N-Fe/Fe3C@C）So that Fe/Fe3C is coated by carbon nanomaterial, it is to avoid Fe/Fe3C is straight
Connect exposure and protect Fe/Fe in the electrolytic solution3The structure and surface stability of C, has on the other hand also well reconciled by Fe/
Fe3C volumetric expansions and the mechanical tension that produces, it is suppressed that Fe/Fe3The polymerization of C, therefore maintains structure and electrical integrity.Cause
This, this electrode material shows very high reversible specific capacity, and high rate performance is all well and good, and particularly stability is fine.It is worth note
Meaning, material and manufacture method all can be prepared on a large scale, for practical application very attractive.
Description of the drawings
Accompanying drawing 1 contains Fe/Fe for the present invention3The state change map of mixed liquor in the preparation method of the carbon nano net of C；
Accompanying drawing 2 contains Fe/Fe for the present invention3The step of carbon nano net preparation method of C schematic diagram；
Accompanying drawing 3 is N-Fe/Fe prepared by the embodiment of the present invention 13The 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 23The multiplying power and cycle performance figure of C@C.
Specific embodiment
The present invention contains Fe/Fe3The preparation method of the carbon nano net of C, it comprises the following steps：（a）Pyrrole monomer is added
Polyreaction is carried out in water obtains polypyrrole ball dispersion liquid；（b）To in the dispersion liquid, add ferrous salt to carry out complex reaction, dry
PPy-Fe coordination compound is obtained afterwards；（c）The PPy-Fe coordination compounds are placed in reducing atmosphere carries out calcining carbonization, such as Fig. 2
Shown.Use a kind of easy method without template to synthesize and include Fe/Fe3The carbon nanometer mesh material of the N doping of C
（Abbreviation N-Fe/Fe3C@C）So that Fe/Fe3C is coated by carbon nanomaterial, it is to avoid Fe/Fe3C is directly exposed in electrolyte
And protect Fe/Fe3The structure and surface stability of C, has on the other hand also well reconciled by Fe/Fe3C volumetric expansions and produce
Raw mechanical tension, it is suppressed that Fe/Fe3The polymerization of C, therefore maintains structure and electrical integrity.Therefore, this electrode material
Very high reversible specific capacity is shown, high rate performance is all well and good, and particularly stability is fine.It should be noted that material and system
Make method all to be prepared on a large scale, for practical application very attractive.
Step（a）In, the polyreaction is in hydrogen peroxide solution and FeCl2·4H2Stir in 0 ~ 30 DEG C under the initiation of O
Reaction 3 ~ 8 hours.Pyrrole monomer, hydrogen peroxide solution, FeCl2·4H2The ratio of O and water is 1 ~ 5ml：8~15ml：0.1~0.5g：
80~150ml.Step（a）In, in water, first add pyrrole monomer, FeCl2·4H2O, subsequent Deca hydrogen peroxide solution are polymerized
Reaction.
Step（b）In, FeCl is added in the dispersion liquid2·4H2O, subsequent Deca hydrogen peroxide solution carry out complex reaction
Dispersion liquid is made within more than 24 hours to become clear as shown in figure 1, dispersion liquid, FeCl2·4H2The ratio of O and hydrogen peroxide solution is 80
~150ml：0.3~0.5g：15~25ml.H in the hydrogen peroxide solution2O2Mass concentration be 20 ~ 35%.
Step（c）In, the reducing atmosphere is that argon and hydrogen are constituted, and its volume flow ratio is 3 ~ 8：1, calcining heat
For 600 ~ 1100 DEG C.
By prepared N-Fe/Fe3C@C, acetylene black, PTFE binding agents are with 7:2:1 mass ratio mixing, is coated in nickel foam and makes
Into electrode, electrode slice is vacuum dried 24h at 60 DEG C as negative pole；With lithium piece as to electrode, the LiPF of 1 mol/L6It is dissolved in
Ethylene carbonate（EC）, methyl ethyl ester（EMC）, diethyl carbonate（DEC）By volume 4:3:3 electrolysis being mixed to form
As electrolyte in liquid, Celgard 2400 is fabricated to button cell as barrier film（CR2025）.
The present invention is further described below in conjunction with accompanying drawing embodiment.
Embodiment 1
The present embodiment provides a kind of using PPy-Fe coordination compounds preparation N-Fe/Fe3C@C nano mesh materials are used as lithium ion
The method of cell negative electrode material, specially：
（a）To in three-neck flask, under room temperature environment, add the H of 88 mL2O, 2 mL pyrroles, 0.2 g FeCl2·4H2O,
Then 10 mL H are slowly added dropwise2O2, stir 6 h；
（b）Add 0.6 g FeCl2·4H2O, is then slowly added dropwise 30 mL H2O2；24 more than h are stirred, solution is gradually
Become clear, in glassy yellow；
（c）By the PPy-Fe coordination compounds vacuum drying；
（d）In Ar (200 sccm) and H in tube furnace2Under the atmosphere of (40 sccm), 900 C calcine 2 h；
（e）By the N-Fe/Fe3C@C nano mesh materials make lithium ion battery negative material；Its scanning electron microscope (SEM) photograph is as schemed
Shown in 3.
Embodiment 2
The present embodiment provides a kind of using PPy-Fe coordination compounds preparation N-Fe/Fe3C@C nano mesh materials are used as lithium ion
Essentially identical in the method for cell negative electrode material, its concrete steps and embodiment 1, except for the difference that reagent quality is different, specifically
For：
（a）To in three-neck flask, under room temperature environment, add the H of 88 mL2O, 2 mL pyrroles, 0.2 g FeCl2·4H2O,
Then 10 mL H are slowly added dropwise2O2.Stir 6 h；
（b）Add 0.34 g FeCl2·4H2O, is then slowly added dropwise 17 mL H2O2.24 more than h are stirred, solution is gradually
Become clear, in glassy yellow；
（c）By the PPy-Fe coordination compounds vacuum drying；
（d）In Ar (200 sccm) and H in tube furnace2Under the atmosphere of (40 sccm), 900 C calcine 2 h；
（e）By the N-Fe/Fe3C@C nano mesh materials make lithium ion battery negative material, and its scanning electron microscope (SEM) photograph is as schemed
Shown in 3, its high rate performance and cycle performance are as shown in Figure 4.
Embodiment 3
The present embodiment provides a kind of using PPy-Fe coordination compounds preparation N-Fe/Fe3C@C nano mesh materials are used as lithium ion
Essentially identical in the method for cell negative electrode material, its concrete steps and embodiment 1, except for the difference that reagent quality is different, specifically
For：
（a）At 0 DEG C, the H of 80 mL is added in three-neck flask2O, 1 mL pyrroles, 0.1 g FeCl2·4H2O, Ran Houhuan
Slow Deca（1 drop/sec）8 mL H2O2（20wt%）, stir 3h；
（b）Add 0.3g FeCl2·4H2O, is then slowly added dropwise 15 mL H2O2；24 more than h are stirred, solution gradually becomes
Clear is obtained, in glassy yellow；
（c）By the PPy-Fe coordination compounds vacuum drying；
（d）In Ar (120 sccm) and H in tube furnace2Atmosphere 5 h of lower 600 DEG C of calcinings of (40 sccm).
Embodiment 4
The present embodiment provides a kind of using PPy-Fe coordination compounds preparation N-Fe/Fe3C@C nano mesh materials are used as lithium ion
Essentially identical in the method for cell negative electrode material, its concrete steps and embodiment 1, except for the difference that reagent quality is different, specifically
For：
（a）At 30 DEG C, the H of 150 mL is added in three-neck flask2O, 5mL pyrroles, 0.5g FeCl2·4H2O, Ran Houhuan
Slow Deca（2 drops/sec）15mL H2O2（35wt%）；Stirring 8h；
（b）Add 0.5 g FeCl2·4H2O, is then slowly added dropwise 25mL H2O2.24 more than h are stirred, solution gradually becomes
Clear is obtained, in glassy yellow；
（c）By the PPy-Fe coordination compounds vacuum drying；
（d）In Ar (320 sccm) and H in tube furnace2Lower 1100 DEG C of the atmosphere of (40 sccm) calcines 1h；
Above-described embodiment technology design only to illustrate the invention and feature, its object is to allow person skilled in the art
Scholar will appreciate that present disclosure and implement according to this, can not be limited the scope of the invention with this, all according to the present invention
Equivalence changes or modification that spirit is made, should all be included within the scope of the present invention.
Claims (8)
1. a kind of containing Fe/Fe3The preparation method of the carbon nano net of C, it is characterised in that it comprises the following steps：
A pyrrole monomer is added to the water by () carries out polyreaction at 0～30 DEG C and obtains polypyrrole ball dispersion liquid；
B () adds FeCl again in the dispersion liquid2·4H2O, subsequent Deca hydrogen peroxide solution carry out complex reaction, after drying
PPy-Fe coordination compounds；Dispersion liquid, FeCl2·4H2The ratio of O and hydrogen peroxide solution is 80～150ml：0.3～0.5g：15～
25ml,
C () is placed in the PPy-Fe coordination compounds in reducing atmosphere and carries out calcining carbonization；The reducing atmosphere is argon
Gas and hydrogen composition, its volume flow ratio is 3～8：1, calcining heat is 600～1100 DEG C.
2. Fe/Fe is contained according to claim 13The preparation method of the carbon nano net of C, it is characterised in that：In step (a), described
Polyreaction is in hydrogen peroxide solution and FeCl2·4H2Stirring reaction 3～8 hours under the initiation of O.
3. Fe/Fe is contained according to claim 23The preparation method of the carbon nano net of C, it is characterised in that：In step (a), pyrroles
Monomer, hydrogen peroxide solution, FeCl2·4H2The ratio of O and water is 1～5ml：8～15ml：0.1～0.5g：80～150ml.
4. Fe/Fe is contained according to claim 33The preparation method of the carbon nano net of C, it is characterised in that：In step (a), first to
Pyrrole monomer, FeCl is added in water2·4H2O, subsequent Deca hydrogen peroxide solution carry out polyreaction.
5. Fe/Fe is contained according to claim 13The preparation method of the carbon nano net of C, it is characterised in that：In step (b), to institute
State addition FeCl in dispersion liquid2·4H2O, subsequent Deca hydrogen peroxide solution carries out complex reaction makes dispersion liquid become clear for more than 24 hours
Clear bright.
6. Fe/Fe is contained according to claim 2 or 43The preparation method of the carbon nano net of C, it is characterised in that：The hydrogen peroxide
H in solution2O2Mass concentration be 20～35%.
7. a kind of containing Fe/Fe3The carbon nano net of C, is prepared from by arbitrary preparation method in claim 1 to 6.
8. Fe/Fe is contained described in claim 73Application of the carbon nano net of C in lithium ion battery negative material.
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Non-Patent Citations (2)
| Title |
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| Core-shell Fe@Fe3C/C nanocomposites as anode materials for Li ion batteries;Liwei Su et al;《Electrochimica Acta》;20120911;第87卷;全文 * |
| Fe-added Fe3C carbon nanofibers as anode for Li ion batteries with excellent low-temperature performance;Jiaxin Li et al;《Electrochimica Acta》;20141203;第153卷;全文 * |
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