CN109742350A - A kind of ferroso-ferric oxide/graphene composite material preparation method of nitridation - Google Patents
A kind of ferroso-ferric oxide/graphene composite material preparation method of nitridation Download PDFInfo
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Abstract
The present invention provides the Fe of nitridation3O4The preparation method of/graphene composite material, which comprises the steps of: use ferrocene for raw material, in 500-600 DEG C of thermal cracking 4-6h, obtain Fe2O3, by Fe2O3It is mixed with graphene oxide according to mass ratio for 5-10:1, Fe is obtained after grinding2O3With the mixture of graphene oxide；By resulting mixture in NH3Under the conditions of flow is 80-100mL/min, in NH3In atmosphere, automatic oxidation reduction reaction and nitrogen treatment are carried out at 500-600 DEG C, after reacting 4-8h, in NH3Cool down in atmosphere with furnace, the Fe nitrogenized3O4/ graphene composite material.Gained Fe3O4‑XNx/Ny- graphene composite material specific surface area with higher is up to 150m2/ g, which has good charge-discharge performance, in 0.1Ag‑1Discharge capacity is 1500mAhg‑1, material stability with higher, after 250 circulations, in 0.5Ag‑1Under be still able to maintain discharge capacity be 850mAhg‑1。
Description
Technical field
The invention belongs to photoelectric fields, are related to a kind of electrode material, specifically Fe3O4- xNx/N- graphene composite wood
The preparation method of material.
Background technique
Carbon material is most widely used lithium ion battery negative material so far, but its maximum deficiency is exactly theoretical
Specific capacity is only 372mAhg-1, it is not able to satisfy requirement of the modern society to portable high-energy mobile power source.Therefore, it seeks new
The alternative materials haveing excellent performance become emphasis.The oxide of transition-metal Fe, Co, Ni, Cu etc. is due to its higher specific capacity
(generally in 700mAhg-1More than), become a kind of lithium ion battery negative material to attract attention.In transition metal oxide
In base lithium ion negative electrode material, Fe3O4It is to compare one of the negative electrode material with application potential, theoretical capacity 926mAh
g-1, it is in addition cheap, it is resourceful and environmentally friendly the features such as make which give great concerns.But four oxidations three
When iron is as electrode material, electron conduction is poor, and biggish volume change can be generated in charge and discharge process, results in
The structure of particle and entire electrode is destroyed, thus cycle life is poor.Again, Fe3O4Magnetic particle is easy to reunite, and reaction is made to live
Property site reduce, so needing to improve Fe3O4Performance.
In the past few years, huge effort has been made to solve these problems, by changing surface topography, reducing
Particle size constructs porous structure and is to synthesize various nanostructures in conjunction with conductive agents such as carbon-based and graphene-based materials
Common method.Recently, the three-dimensional grapheme network structure containing metal oxide is caused extensively due to its unique performance
General concern.Application number CN 106935830A discloses a kind of lithium ion battery composite cathode material and preparation method thereof and answers
With.Li [Ni disclosed in this application1-x-yCoxMny]O2/ three-dimensional grapheme positive electrode possesses bigger capacity, prepares the anode
The method of material is easy to operate, but there is no obvious for the lithium ion battery chemical property prepared in the technical method
It improves, there are certain limitations.Application number CN107293710A discloses a kind of transition metal oxide/graphene composite wood
The preparation method of material.The good cycling stability for the lithium ion battery that this method is prepared, but battery capacity is slightly inadequate.Highest
Be sesquioxide/graphene composite material, battery capacity is in 1252.7mAhg-1, however ferric oxide composite material is in height
Current density and synthesis complex condition, cyclical stability are poor.
Summary of the invention
, loop attenuation low as initial coulomb efficiency existing for electrode anode material for ferroso-ferric oxide be fast and multiplying power
The disadvantage of performance difference, the object of the present invention is to provide improve charge-discharge performance of the ferroso-ferric oxide as electrode anode material.
In order to achieve the above object, the present invention provides a kind of Fe of nitridation3O4The preparation side of/graphene composite material
Method.Innovative proposition of the invention embeds four iron oxide, electric conductivity on the one hand can be improved, separately to nitrogenize graphene as carrier
On the one hand Fe is solved3O4Bulk effect, and provide its specific preparation method, oxygen is mainly utilized in this kind of preparation method
Change the mode of iron progress synchronous with the nitrogenation treatment technology of the reaction of the automatic oxidation reduction of graphene oxide and ammonia, preparation method
Simply, easily operated.Innovative proposing of the invention synthesizes Fe with graphite thermal method3O4/ graphene nanocomposite material,
Fe3O4/ graphene combination electrode has good cyclical stability in charge and discharge cycles.
The Fe of nitridation of the invention3O4The preparation method of/graphene composite material, which comprises the steps of:
It uses ferrocene for raw material, in 500-600 DEG C of thermal cracking 4-6h, obtains Fe2O3, by Fe2O3With graphene oxide according to quality
Than mixing for 5-10:1, Fe is obtained after grinding2O3With the mixture of graphene oxide；By resulting mixture in NH3Flow is
Under the conditions of 80-100mL/min, in NH3In atmosphere, automatic oxidation reduction reaction and nitrogen treatment, reaction are carried out at 500-600 DEG C
After 4-8h, in NH3Cool down in atmosphere with furnace, the Fe nitrogenized3O4/ graphene composite material.
Preferably, the Fe of the nitridation3O4The molecular formula of/graphene composite material is Fe3O4-XNx/Ny- graphene,
Wherein, x=0.1-0.25, y=1%-8%.
Preferably, the graphene oxide is prepared in improved hummer method.
Preferably, the nitrogen treatment and automatic oxidation reduction process occur simultaneously.
Preferably, the Fe of resulting nitridation3O4The specific surface area of/graphene composite material reaches 150m2/ g or more.
Preferably, the Fe of resulting nitridation3O4/ graphene composite material is in 0.1Ag-1Discharge capacity is 1500mAhg-1,
After crossing 250 circulations, in 0.5Ag-1Under be still able to maintain discharge capacity be 850mAhg-1。
The present invention first passes through the Fe that thermal-cracking method obtains morphology controllable2O3, and by with graphene oxide to iron oxide
Class carbon thermal reduction effect, by Fe2O3It is reduced to Fe3O4, and graphene oxide carries out autoreduction during heating and is formed
Graphene.Meanwhile in ammonia atmosphere, in the dynamic process of reduction reaction, Fe3O4Nitrogen source is introduced with graphene surface, is formed
The Fe of nitridation3O4/ graphene composite material.Such automatic oxidation reduction reaction and nitrogenation treatment technology, so that nanoscale nitrogenizes
Fe3O4Particle is encapsulated in space and is dispersed on the surface of nitridation graphene nanometer sheet, this not only effectively promotes two
Electron-transport between person enhances the conductivity of the compound comprising the two also significantly.On the one hand this kind of composite material be
It, can be in the case where not destroying internal carbon internal structure with outer since the carbon atomic layer of single layer has very strong flexibility
The change of power and generate deformation, to keep the stability of its structure, such result shows it in terms of electrochemistry
Excellent electrode is forthright again and stability, this is primarily due on (1) graphene film, and there are a large amount of oxygen-containing functional group Fe3O4It receives
Rice material can be compound with graphene by chemical bond, prevents falling off and damaging for material in reaction process；(2) graphite is nitrogenized
Good electric conductivity possessed by alkene itself can guarantee good electrochemical contact between ferriferrous oxide particles, and graphene sheet layer
Between interaction can form tridimensional nano net structure, reduce contact resistance to improve electrochemistry moderate multiplying factor performance.
These advantages make such combination electrode have great application value on lithium ion battery anode material.
The invention proposes utilize iron oxide to react with the automatic oxidation reduction of graphene oxide and the nitrogen treatment work of ammonia
The synchronous mode carried out of skill, realizes the Fe of nitrogen treatment3O4With the preparation of graphene composite material.Its preparation process is simple,
Easily operated, products obtained therefrom large specific surface area, specific capacity is big, and stability is high.
The present invention is compared with having invention, and progress is significant.The present invention takes full advantage of iron oxide and graphene oxide
Automatic oxidation reduction reaction, and realize the process of nitridation simultaneously.The Fe of gained nitridation3O4/ graphene composite material has higher
Specific surface area up to 150m2/ g, which has good charge-discharge performance, in 0.1Ag-1Discharge capacity is
1500mAhg-1, material stability with higher, after 250 circulations, in 0.5Ag-1Under be still able to maintain discharge capacity and be
850mAhg-1。
Detailed description of the invention
The SEM of Fig. 1 embodiment 1 schemes；
The TEM of Fig. 2 embodiment 2 schemes；
The TEM of Fig. 3 embodiment 3 schemes；
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, this field skill
Art personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims
Limited range.
Graphene oxide in following embodiment is prepared using improved hummer method, method particularly includes:
Step a) weighs 0.6g graphite and 1.0g NaNO respectively3It is put into the beaker of 250ml, in ice-water bath and stirring
Under the conditions of be slowly added to 35ml mass concentration be (95~98%) H2SO4Stir 1h；
Step b) is slowly added to 3gKMnO4, 1h adds, and continues to stir 4h；
Step c) removes ice-water bath, is warming up to 35 DEG C, continues to stir 30min.150ml distilled water is slowly added to, is terminated
After be warming up to 98 DEG C, stir 15min.
Step d) preheats 200ml pure distilled water under the conditions of 60 DEG C in advance, and solution reacted in step c) is being stirred
Under the conditions of be poured slowly into hot water, then by 10ml mass concentration (30%) H2O2It is added in solution.Solution becomes yellow at this time, quiet
It sets overnight.
Step e) centrifuge washing, obtains graphene oxide.
Embodiment 1
A kind of Fe of nitridation3O4The preparation method of/graphene composite material, specific steps are as follows:
(1) using ferrocene as raw material, Fe is prepared in 600 DEG C of thermal cracking 4h2O3；
(2) graphene oxide is prepared according to the improved hummer method；
(3) by Fe obtained by (1) (2)2O3It is mixed with graphene oxide according to mass ratio for 8:1, Fe is obtained after grinding2O3With
The mixture of graphene oxide.
(4) by uniform mixture obtained by (3) in NH3Under the conditions of flow is 80mL/min, in NH3In atmosphere, at 500 DEG C
Down while automatic oxidation reduction reaction and nitrogen treatment are carried out, after reacting 6h, in NH3Cool down in atmosphere with furnace, is nitrogenized
Fe3O4/ graphene composite material.
(5) using the content of ICP detection Fe, using the content of the N in elemental analysis and XPS quantitative analysis composite material,
Utilize the content of XPS monitoring O.The molecular formula of gained composite material in embodiment are as follows: (Fe3O3.85N0.15/N0.05Graphene).
Use nitrogen adsorption desorption method BET method test specific surface area for 180.5m2/g。
SEM morphology analysis is carried out to gained sample using the Hitachi S-4800II of Japan, finds prepared nitridation
Fe3O4In the spindle bodily form, size about 50nm is uniformly distributed on the surface of graphene.
By the Fe of resulting nitridation3O4/ graphene composite material and acetylene black and ((25 DEG C of specific gravity of ptfe emulsion
1.52g/cm3, solid content 60%) and mixing weighed with mass ratio 8:2:1, coated on the porous nickel mesh handled well, flattens and dry
It is dry to carry out electrochemical property test.The composite material has good charge-discharge performance, in 0.1Ag-1Discharge capacity is
1200mAhg-1, material stability with higher, after 250 circulations, in 0.5Ag-1Under be still able to maintain discharge capacity and be
780mAhg-1。
Embodiment 2
A kind of Fe of nitridation3O4The preparation method of/graphene composite material, specific steps are as follows:
(1) using ferrocene as raw material, Fe is prepared in 500 DEG C of thermal cracking 4h2O3；
(2) graphene oxide is prepared according to the improved hummer method；
(3) by Fe obtained by (1) (2)2O3It is mixed with graphene oxide according to mass ratio for 7:1, Fe is obtained after grinding2O3With
The mixture of graphene oxide.
(4) by uniform mixture obtained by (3) in NH3Under the conditions of flow is 100mL/min, in NH3In atmosphere, at 600 DEG C
Down while automatic oxidation reduction reaction and nitrogen treatment are carried out, after reacting 4h, in NH3Cool down in atmosphere with furnace, is nitrogenized
Fe3O4/ graphene composite material.
(5) using the content of ICP detection Fe, using the content of the N in elemental analysis and XPS quantitative analysis composite material,
Utilize the content of XPS monitoring O.The molecular formula of gained composite material in embodiment are as follows: (Fe3O3.80N0.2/N0.05Graphene).
Use nitrogen adsorption desorption method BET method test specific surface area for 200.2m2/g。
TEM morphology analysis is carried out to gained sample using the Hitachi S-4800II of Japan, discovery diameter dimension is about
The Fe of the nitridation of 60nm3O4Nanometer spherical distribution of particles is on the surface of graphene.
By the Fe of resulting nitridation3O4/ graphene composite material and acetylene black and (25 DEG C of specific gravity of ptfe emulsion
1.52g/cm3, solid content 60%) and mixing weighed with mass ratio 8:2:1, coated on the porous nickel mesh handled well, flattens and dry
It is dry to carry out electrochemical property test.The composite material has good charge-discharge performance, in 0.1Ag-1Discharge capacity is
1500mAhg-1, material stability with higher, after 250 circulations, in 0.5Ag-1Under be still able to maintain discharge capacity and be
850mAhg-1。
Embodiment 3
A kind of Fe of nitridation3O4The preparation method of/graphene composite material, specific steps are as follows:
(1) using ferrocene as raw material, Fe is prepared in 550 DEG C of thermal cracking 5h2O3；
(2) graphene oxide is prepared according to the improved hummer method；
(3) by Fe obtained by (1) (2)2O3It is mixed with graphene oxide according to mass ratio for 6:1, Fe is obtained after grinding2O3With
The mixture of graphene oxide.
(4) by uniform mixture obtained by (3) in NH3Under the conditions of flow is 90mL/min, in NH3In atmosphere, at 550 DEG C
Down while automatic oxidation reduction reaction and nitrogen treatment are carried out, after reacting 8h, in NH3Cool down in atmosphere with furnace, is nitrogenized
Fe3O4/ graphene composite material.
(5) using the content of ICP detection Fe, using the content of the N in elemental analysis and XPS quantitative analysis composite material,
Utilize the content of XPS monitoring O.The molecular formula of gained composite material in embodiment are as follows: (Fe3O3.72N0.28/N0.06Graphene).
Use ammonia adsorption desorption method BET method test specific surface area for 160m2/g。
Using Japan Hitachi S-4800II to gained sample carry out TEM morphology analysis, discovery nitridation Fe3O4 with
Aggregate form exists, and is laid on the surface of graphene.But it examines, it can be found that aggregate is small by many nanometers
Particle is constituted.
By composite material and acetylene black and ptfe emulsion (25 DEG C of 1.52g/cm of specific gravity3, solid content 60%) with
Mass ratio 8:2:1 weighs mixing, carries out electrochemical property test coated in drying on the porous nickel mesh handled well, is flattened.This is multiple
Condensation material has good charge-discharge performance, in 0.1Ag-1Discharge capacity is 1300mAhg-1, material stabilization with higher
Property, after 250 circulations, in 0.5Ag-1Under be still able to maintain discharge capacity be 840mAhg-1。
Embodiment 4
A kind of Fe of nitridation3O4The preparation method of/graphene composite material, specific steps are as follows:
(1) using ferrocene as raw material, Fe is prepared in 600 DEG C of thermal cracking 4h2O3；
(2) graphene oxide is prepared according to the improved hummer method；
(3) by Fe obtained by (1) (2)2O3It is mixed with graphene oxide according to mass ratio for 6:1, Fe is obtained after grinding2O3With
The mixture of graphene oxide.
(4) by uniform mixture obtained by (3) in NH3Under the conditions of flow is 90mL/min, in NH3In atmosphere, at 550 DEG C
Down while automatic oxidation reduction reaction and nitrogen treatment are carried out, after reacting 6h, in NH3Cool down in atmosphere with furnace, is nitrogenized
Fe3O4/ graphene composite material.
(5) using the content of ICP detection Fe, using the content of the N in elemental analysis and XPS quantitative analysis composite material,
Utilize the content of XPS monitoring O.The molecular formula of gained composite material in embodiment are as follows: (Fe3O3.67N0.33/N0.06Graphene).
Nitrogen is used to inhale de- method BET method test specific surface area for 190.2m2/g。
SEM morphology analysis is carried out to gained sample using the Hitachi S-4800II of Japan.It was found that nitridation Fe3O4In ball
Shape, particle size are about 55nm, and monodisperse is on the surface of graphene.
Composite material and acetylene black and ptfe emulsion (25 DEG C of 1.52g/cm of specific gravity3, solid content 60%) and with matter
Amount weighs mixing than 8:2:1, carries out electrochemical property test coated in drying on the porous nickel mesh handled well, is flattened.This is compound
Material has good charge-discharge performance, in 0.1Ag-1Discharge capacity is 1425mAhg-1, material stability with higher,
After 250 circulations, in 0.5Ag-1Under be still able to maintain discharge capacity be 835mAhg-1。
Claims (6)
1. a kind of Fe of nitridation3O4The preparation method of/graphene composite material, which comprises the steps of: use two
Luxuriant iron obtains Fe in 500-600 DEG C of thermal cracking 4-6h for raw material2O3, by Fe2O3With graphene oxide according to mass ratio be 5-
10:1 mixing, obtains Fe after grinding2O3With the mixture of graphene oxide；By resulting mixture in NH3Flow is 80-
Under the conditions of 100mL/min, in NH3In atmosphere, automatic oxidation reduction reaction and nitrogen treatment are carried out at 500-600 DEG C, react 4-8h
Afterwards, in NH3Cool down in atmosphere with furnace, the Fe nitrogenized3O4/ graphene composite material.
2. the Fe nitrogenized as described in claim 13O4The preparation method of/graphene composite material, which is characterized in that described
The Fe of nitridation3O4The molecular formula of/graphene composite material is Fe3O4-XNx/Ny- graphene, wherein x=0.1-0.25, y=
1%-8%.
3. the Fe nitrogenized as described in claim 13O4The preparation method of/graphene composite material, which is characterized in that described
Graphene oxide is prepared in improved hummer method.
4. the Fe nitrogenized as described in claim 13O4The preparation method of/graphene composite material, which is characterized in that described
Nitrogen treatment and automatic oxidation reduction process occur simultaneously.
5. the Fe nitrogenized as described in claim 13O4The preparation method of/graphene composite material, which is characterized in that resulting
The Fe of nitridation3O4The specific surface area of/graphene composite material reaches 150m2/ g or more.
6. the Fe nitrogenized as described in claim 13O4The preparation method of/graphene composite material, which is characterized in that resulting
The Fe of nitridation3O4/ graphene composite material is in 0.1Ag-1Discharge capacity is 1500mAhg-1, after crossing 250 circulations, in 0.5Ag-1
Under be still able to maintain discharge capacity be 850mAhg-1。
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Application publication date: 20190510 Assignee: SHANGHAI SUPERHIGH ENVIRONMENTAL PROTECTION TECHNOLOGY CO.,LTD. Assignor: SHANGHAI INSTITUTE OF TECHNOLOGY Contract record no.: X2022310000095 Denomination of invention: A kind of preparation method of nitrided ferric oxide/graphene composite material Granted publication date: 20211119 License type: Common License Record date: 20220829 |