CN108110231A - A kind of carbon coating Fe4N nanocomposites, preparation method and applications - Google Patents
A kind of carbon coating Fe4N nanocomposites, preparation method and applications Download PDFInfo
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- CN108110231A CN108110231A CN201711265934.8A CN201711265934A CN108110231A CN 108110231 A CN108110231 A CN 108110231A CN 201711265934 A CN201711265934 A CN 201711265934A CN 108110231 A CN108110231 A CN 108110231A
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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
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- 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 present invention provides a kind of carbon coating Fe for ion cathode material lithium4N nanocomposites, preparation method and applications.The carbon coating Fe4The size of N nanocomposites is 30 100nm, and the thickness of carbon coating layer is 5 10nm.Method includes：By dicyandiamide and FeCl3·6H2The solution that O dissolvings are uniformly mixed, heating evaporating water obtain dicyandiamide and FeCl3·6H2The mixture of O, the temperature reaction in tube furnace obtain Fe after cooling4N powder coats Fe using glucose4N powder obtains carbon coating Fe after carbonization4N nanometer combined electrode materials.This method manufacturing cost is low, simple for process, the carbon coating Fe being prepared4N nanocomposite patterns are homogeneous, for ion cathode material lithium, have good storage lithium performance, cycle life and high rate performance.
Description
Technical field
The present invention relates to novel energy resource material technology fields, and in particular to a kind of carbon bag for lithium ion battery negative material
Cover Fe4N nanocomposites, preparation method and its application in lithium ion battery negative material.
Background technology
Lithium ion battery due to its high-energy, high power density, high security and it is environmental-friendly the features such as it is extensive
For fields such as mobile electronic device energy storage.At present, for lithium ion battery research just towards high-energy or power density, compared with
Good cryogenic property and the direction of the power battery material of high rate capability are developed.Existing lithium ion battery negative material master
If carbon negative pole material, but due to the theoretical capacity of commercial graphite cathode relatively low (372mAh/g), poor high rate performance,
The S EI films (solid electrolyte film) that first charge-discharge is formed greatly cause the loss of capacity and easily safety problem etc. are triggered to lack
Point strongly limits the application in high power density type power battery field.In order to develop a kind of high-energy density and high safety
Property lithium ion battery negative material meet the needs of high power type power battery, realize higher economic benefits, social benefit
And the development strategy deployment of country, so there is an urgent need to find the substitute of graphite cathode material.The spy of new electrode materials
Rope is most important for developing the rechargeable lithium ion batteries with high power capacity and excellent stability.Graphite cathode material at present
Substitute includes modified graphite, Si sills, Sn sills and MnXmType (M is transition metal, X be it is nonmetallic including O, S, N, P,
B or polymer) material.For MnXmThe storage lithium mechanism of section bar material resolves into M for active material portion or completely reversibility0And phase
The lithium salts answered, wherein can be expressed simply as
Transition metal nitride due to its with excellent chemical property, high chemical stability and be expected to be applied to power
In cell negative electrode material.The specific electronic structure of transition elements (IIIB-VIII races) is characterized in that valence electron can take up portion
Divide the d tracks of filling, because energy level of the electronics between 4s and 3d, 5s and 4d or 6s and 5d approaches.When nitride participates in
During redox reaction, multivalent state is generated effectively to store energy.However up to the present, the nitride as active material
Practical application is far from, this is because its larger volume expansion causes the capacity during electrochemical reaction is cycled quickly to decline
Subtract.
The content of the invention
To solve the above-mentioned problems, the present invention provides a kind of carbon coating Fe4N nanocomposites, preparation method and its
In the application of lithium ion battery negative material.By by Fe4N active materials are reduced in size to nanoscale, shorten lithium ion
Diffusion path and storage time and the cycling for effectively reducing mechanical stress to adapt to the variation of different volumes and improve electrode material
Ability, also, by by Fe4N active materials are compounded to form carbon coating structure with carbon, it is prevented to be reacted with electrolyte, and protection is lived
Property substance Fe4N, improves the stability of material, while inhibits its Volumetric expansion and Fe4The shortcomings of N easily reunites, also, carbon
There is the variation of buffers active substance excess volume during embedding lithium/de- lithium is cycled, carbon material is due to the lithium of its own
Ion storage ability and have certain contribution to the promotion of battery capacity, the compound electric conductivity for improving electrode of carbon and contribute to
By the electron transmission generated during the redox reaction of active material to collector, so as to improve as lithium ion battery
Cycle performance and high rate performance during negative material.
The present invention adopts the following technical scheme that：
A kind of carbon coating Fe4N nanocomposites, the Fe4The surface of N particles has carbon coating layer, the carbon coating layer
Thickness be 5-10nm, carbon coating Fe4The size of N nanocomposites is 30-100nm.
A kind of carbon coating Fe4The preparation method of N nanocomposites, this method comprises the following steps：
(1) by dicyandiamide and FeCl3·6H2O is dissolved in deionized water, with magnetic stirrer, is uniformly mixed
Solution
(2) solution obtained to step (1) heats, until the moisture in solution is evaporated completely, obtain dicyandiamide with
FeCl3·6H2The mixture of O；
(3) mixture obtained by step (2) is placed in porcelain boat, be positioned in tube furnace, is warming up under argon atmosphere
850-950℃；
(4) when the reaction tube internal temperature in tube furnace reaches 850-950 DEG C, argon gas is closed, is passed through into reaction tube
Ammonia, the temperature in reaction tube continue to be increased to 950-1050 DEG C, when keeping 1-2 small, are continually fed into ammonia until tube furnace drops
To room temperature, the powder for collecting brown on porcelain boat obtains Fe4N；Wherein, ammonia flow velocity is 80-120mL/min；
(5) Fe for obtaining step (4)4N powder is with glucose according to 1：The mass ratio of (1-8) is dissolved in deionized water,
After when mechanical agitation 3-5 is small, final solution is transferred in polytetrafluoroethylliner liner reaction kettle, is positioned in drying box, in
When 160-200 DEG C of heat preservation 8-12 is small, Fe is coated by centrifuging and being dried to obtain glucose4The powder of N；
(6) powder that step (5) obtains is placed in tube furnace, heat up carbonization under the atmosphere of argon gas, finally obtains carbon
Coat Fe4N nanocomposites.
Preferably, in step (1), dicyandiamide, FeCl3·6H2O and the mass ratio of deionized water are (5-10)：(3-5)：
(250-350).Preferably, in step (3), argon gas flow velocity is 60-100mL/min.
Preferably, in step (3), 900 DEG C are warming up under argon atmosphere.
Preferably, in step (4), the temperature in reaction tube continues to be increased to 1000 DEG C, when holding 1.5 is small.
Preferably, in step (5), when 180 DEG C of heat preservations 10 are small.
Preferably, in step (6), in tube furnace, be warming up under the atmosphere of argon gas 500-900 DEG C maintain 1-2 it is small when
It is carbonized, it is furthermore preferred that when carbonization time is that 800 DEG C of maintenances 1 are small.
The carbon coating Fe that the present invention is prepared4N nanocomposites, Fe4The surface of N nano particles has carbon coating layer,
The thickness of the carbon coating layer is 5-10nm, carbon coating Fe4The size of N nanocomposites is 30-100nm.
Carbon coating Fe of the present invention4N nanocomposites are used for lithium ion battery negative material, are cycled through electrical property
Testing experiment shows there is good storage lithium performance, cycle life and high rate performance：After charging and discharging cycle 100 times, material
The specific capacity of material remains at more than 730mAh/g；Also, high rate performance experiments have shown that, the material is in high current density
After carrying out multiple charge and discharge under 100mA/g, the high reversible capacity of more than 740mAh/g is still kept, the material is in high magnification charge and discharge
Invertibity is good after electricity.
Compared with prior art, the present invention with advantageous effect following prominent：
(1) present invention prepares carbon coating Fe by hydro-thermal method and high temperature pyrolytic cracking (HTP)4It is prepared by N composite nano materials, production
It is at low cost, it is simple for process, it is easy to control；
(2) the carbon coating Fe that the present invention is prepared4N nanocomposite patterns are homogeneous, Fe4The surface tool of N nano particles
There is carbon coating layer, the thickness of the carbon coating layer is 5-10nm, carbon coating Fe4The size of N nanocomposites is 30-100nm
, by the way that active material is reduced to nanoscale, the diffusion path and storage time of lithium ion are shortened, effectively reducing machinery should
Power significantly improves the circulation ability of electrode material to adapt to the variation of different volumes；
(3) present invention is by by Fe4N active materials are compounded to form carbon coating structure with carbon, it is prevented to be reacted with electrolyte,
Protection activity substance Fe4N, improves the stability of material, while inhibits its Volumetric expansion and Fe4The shortcomings of N easily reunites；
(4) the carbon coating Fe that the present invention is prepared4N nanocomposites have good for ion cathode material lithium
Storage lithium performance, cycle life and high rate performance, electrical property loop test experiments have shown that：After charging and discharging cycle 100 times,
Specific capacity remains at more than 730mAh/g；And high rate performance experiments have shown that, the material carries out more at higher current densities
After secondary charge and discharge, the reversible capacity of more than 740mAh/g is still kept, i.e., the invertibity of material is good after high power charging-discharging.
Description of the drawings
Fig. 1 is Fe4The XRD diagram of N materials；
Fig. 2 is carbon coating Fe of the present invention4The TEM figures of N composite nano materials, (a) and (b) is respectively carbon coating Fe4N is compound
Low power and high-resolution the projection figure of nano material；
Fig. 3 is carbon coating Fe of the present invention4Cycle performance when N composite nano materials are as lithium ion battery negative material
Figure；
Fig. 4 is carbon coating Fe of the present invention4High rate performance when N composite nano materials are as lithium ion battery negative material
Figure.
Specific embodiment
Embodiment 1：
(1) by dicyandiamide and FeCl3·6H2O is dissolved in deionized water, with magnetic stirrer 4h, is uniformly mixed
Solution, wherein dicyandiamide, FeCl3·6H2O and the mass ratio of deionized water are 5：3：250；
(2) solution obtained to step (1) heats, until the moisture in solution is evaporated completely, obtain dicyandiamide with
FeCl3·6H2The mixture of O；
(3) mixture obtained by step (2) is placed in porcelain boat, be positioned in tube furnace, be 60mL/min's in flow velocity
850 DEG C are warming up under argon atmosphere；
(4) when the reaction tube internal temperature in tube furnace reaches 850 DEG C, argon gas is closed, 80mL/ is passed through into reaction tube
The ammonia of min, the temperature in reaction tube continue to be increased to 950 DEG C, and continue 2 it is small when, it is still 80mL/min to be continually fed into flow velocity
Ammonia until tube furnace is down to room temperature, the powder for collecting brown on porcelain boat can obtain Fe4N；
(5) Fe for obtaining step (4)4N is with glucose according to 1：1 mass ratio is dissolved in deionized water, mechanical agitation 3
After hour, final solution is transferred in polytetrafluoroethylliner liner reaction kettle, is positioned in drying box, in 160 DEG C of heat preservations
12 it is small when, by centrifuge and be dried to obtain glucose coat Fe4The powder of N；
(6) powder that step (5) obtains is placed in tube furnace, be warming up under the atmosphere of argon gas 500 DEG C maintain 2 it is small when
It is carbonized, finally obtains carbon coating Fe4N composite materials.
Embodiment 2：
(1) by dicyandiamide and FeCl3·6H2O is dissolved in deionized water, with magnetic stirrer 4h, is uniformly mixed
Solution, wherein dicyandiamide, FeCl3·6H2O and the mass ratio of deionized water are 6：4：280；
(2) solution obtained to step (1) heats, until the moisture in solution is evaporated completely,
Obtain dicyandiamide and FeCl3·6H2The mixture of O；
(3) mixture obtained by step (2) is placed in porcelain boat, be positioned in tube furnace, be 80mL/min's in flow velocity
900 DEG C are warming up under argon atmosphere；
(4) when the reaction tube internal temperature in tube furnace reaches 900 DEG C, argon gas is closed, is passed through into reaction tube
The ammonia of 100mL/min, the temperature in reaction tube continue to be increased to 1000 DEG C, and continue 1.5 it is small when, being continually fed into flow velocity is still
For the ammonia of 100mL/min until tube furnace is down to room temperature, the powder for collecting brown on porcelain boat can obtain Fe4N；
(5) Fe for obtaining step (4)4N is with glucose according to 1：2 mass ratio is dissolved in deionized water, mechanical agitation 4
After hour, final solution is transferred in polytetrafluoroethylliner liner reaction kettle, is positioned in drying box, in 180 DEG C of heat preservations
10 it is small when, by centrifuge and be dried to obtain glucose coat Fe4The powder of N；
(6) powder that step (5) obtains is placed in tube furnace, be warming up under the atmosphere of argon gas 600 DEG C maintain 1 it is small when
It is carbonized, finally obtains carbon coating Fe4N composite materials.
Embodiment 3：
(1) by dicyandiamide and FeCl3·6H2O is dissolved in deionized water, with magnetic stirrer 4h,
The solution being uniformly mixed, wherein dicyandiamide, FeCl3·6H2O and the mass ratio of deionized water are 8：5：300；
(2) solution obtained to step (1) heats, until the moisture in solution is evaporated completely,
Obtain dicyandiamide and FeCl3·6H2The mixture of O；
(3) mixture obtained by step (2) is placed in porcelain boat, be positioned in tube furnace, be 100mL/min's in flow velocity
950 DEG C are warming up under argon atmosphere；
(4) when the reaction tube internal temperature in tube furnace reaches 950 DEG C, argon gas is closed, is passed through into reaction tube
The ammonia of 120mL/min, the temperature in reaction tube continue to be increased to 1050 DEG C, and continue 1 it is small when, being continually fed into flow velocity is still
For the ammonia of 120mL/min until tube furnace is down to room temperature, the powder for collecting brown on porcelain boat can obtain Fe4N；
(5) Fe for obtaining step (4)4N is with glucose according to 1：4 mass ratio is dissolved in deionized water, mechanical agitation 5
After hour, final solution is transferred in polytetrafluoroethylliner liner reaction kettle, is positioned in drying box, 8 are kept the temperature in 200 DEG C
Hour, coat Fe by centrifuging and being dried to obtain glucose4The powder of N；
(6) powder that step (5) obtains is placed in tube furnace, be warming up under the atmosphere of argon gas 800 DEG C maintain 1 it is small when
It is carbonized, finally obtains carbon coating Fe4N composite materials.
Embodiment 4：
(1) by dicyandiamide and FeCl3·6H2O is dissolved in deionized water, with magnetic stirrer 4h, is uniformly mixed
Solution, wherein dicyandiamide, FeCl3·6H2O and the mass ratio of deionized water are 10：5：350；
(2) solution obtained to step (1) heats, until the moisture in solution is evaporated completely, obtain dicyandiamide with
FeCl3·6H2The mixture of O；
(3) mixture obtained by step (2) is placed in porcelain boat, be positioned in tube furnace, be 80mL/min's in flow velocity
900 DEG C are warming up under argon atmosphere；
(4) when the reaction tube internal temperature in tube furnace reaches 900 DEG C, argon gas is closed, is passed through into reaction tube
The ammonia of 100mL/min, the temperature in reaction tube continue to be increased to 1000 DEG C, and continue 1.5 it is small when, being continually fed into flow velocity is still
For the ammonia of 100mL/min until tube furnace is down to room temperature, the powder for collecting brown on porcelain boat can obtain Fe4N；
(5) Fe for obtaining step (4)4N is with glucose according to 1：8 mass ratio is dissolved in deionized water, mechanical agitation 4
After hour, final solution is transferred in polytetrafluoroethylliner liner reaction kettle, is positioned in drying box, in 180 DEG C of heat preservations
10 it is small when, by centrifuge and be dried to obtain glucose coat Fe4The powder of N；
(6) powder that step (5) obtains is placed in tube furnace, be warming up under the atmosphere of argon gas 900 DEG C maintain 1 it is small when
It is carbonized, finally obtains carbon coating Fe4N composite materials.
Further, the carbon coating Fe embodiment of the present invention being prepared4N composite materials carry out tem observation analysis,
Middle Fig. 2 (a) and Fig. 2 (b) are respectively carbon coating Fe4Low power and high-resolution the projection figure of N composite nano materials, it is seen that institute of the present invention
The carbon coating Fe being prepared4N composite materials are nanostructured, and pattern is homogeneous, Fe4The surface of N nano particles has carbon coating
Layer, the thickness of the carbon coating layer is 5-10nm, carbon coating Fe4The size of N nanocomposites is 30-100nm.
Further, the carbon coating Fe embodiment of the present invention being prepared4N nanocomposites are used for lithium-ion electric
Pond negative material, carries out electrical property loop test experiment, result of the test cycle performance figure as shown in Figure 3 and shown in Fig. 4 times
Rate performance map, with good storage lithium performance, cycle life and high rate performance：After being charged and discharged 100 times, specific capacity is still
Be maintained at more than 730mAh/g, material of the present invention shown in Fig. 4 different current densities for 100mA/g, 200mA/g, 500mA/g,
Corresponding reversible capacity is respectively 766mAh/g, 665mAh/g, 475mAh/ under 1000mA/g and 100mA/g, after multiple charge and discharge
G, 250mAh/g and 746mAh/g, it is seen that after the material carries out multiple charge and discharge at higher current densities, still keep higher
Reversible capacity, i.e., described material still keeps higher reversible capacity in high power charging-discharging, and the invertibity of material is good.
Invention described above specific embodiment, is not intended to limit the scope of the present invention..It is any this
Modifications, equivalent substitutions and improvements made within the spirit and principle of invention etc., should be included in the claim of the present invention
Within protection domain.
Claims (9)
1. a kind of carbon coating Fe for lithium ion battery negative material4N nanocomposites, it is characterised in that：Fe4N particles
Surface has carbon coating layer, and the thickness of the carbon coating layer is 5-10nm, carbon coating Fe4The size of N nanocomposites is 30-
100nm。
2. a kind of prepare carbon coating Fe described in claim 14The method of N nanocomposites, it is characterised in that：Including walking as follows
Suddenly：
(1) by dicyandiamide and FeCl3·6H2O is dissolved in deionized water, and with magnetic stirrer, what is be uniformly mixed is molten
Liquid；
(2) solution obtained to step (1) heats, until the moisture in solution is evaporated completely, obtain dicyandiamide with
FeCl3·6H2The mixture of O；
(3) mixture obtained by step (2) is placed in porcelain boat, be positioned in tube furnace, 850- is warming up under argon atmosphere
950℃；
(4) when the reaction tube internal temperature in tube furnace reaches 850-950 DEG C, argon gas is closed, ammonia is passed through into reaction tube,
Temperature in reaction tube continues to be increased to 950-1050 DEG C, when keeping 1-2 small, is continually fed into ammonia until tube furnace is down to room
Temperature, the powder for collecting brown on porcelain boat obtain Fe4N；Wherein, ammonia flow velocity is 80-120mL/min；
(5) Fe for obtaining step (4)4N powder is with glucose according to 1：The mass ratio of (1-8) is dissolved in deionized water, and machinery stirs
Mix 3-5 it is small when after, final solution is transferred in polytetrafluoroethylliner liner reaction kettle, is placed in drying box, in 160-200
DEG C heat preservation 8-12 it is small when, by centrifuge and be dried to obtain glucose coat Fe4The powder of N；
(6) powder that step (5) obtains is placed in tube furnace, heat up carbonization under the atmosphere of argon gas, finally obtains carbon coating
Fe4N nanocomposites.
3. according to the method described in claim 2, it is characterized in that：In step (1), dicyandiamide, FeCl3·6H2O and deionization
The mass ratio of water is (5-10)：(3-5)：(250-350).
4. according to the method in claim 2 or 3, it is characterised in that：In step (3), argon gas flow velocity is 60-100mL/min,
900 DEG C are warming up under argon atmosphere.
5. according to the method in claim 2 or 3, it is characterised in that：In step (4), the temperature in reaction tube continues to raise
To 1000 DEG C, when holding 1.5 is small.
6. according to the method in claim 2 or 3, it is characterised in that：It in step (5), is placed in drying box, in 180 DEG C
Keep the temperature 10 it is small when.
7. according to the method in claim 2 or 3, it is characterised in that：In step (6), 500-900 DEG C of maintenance 1-2 is warming up to
Hour is carbonized, it is furthermore preferred that when carbonization time is that 800 DEG C of maintenances 1 are small.
8. according to the method in claim 2 or 3, it is characterised in that：The carbon coating Fe being prepared4N nanocomposites,
Fe4The surface of N nano particles has carbon coating layer, and the thickness of the carbon coating layer is 5-10nm, carbon coating Fe4The nano combined materials of N
The size of material is 30-100nm.
9. a kind of carbon coating Fe described in claim 14The application of N nanocomposites, it is characterised in that：For lithium ion battery
Negative material, after charge and discharge cycles 100 times, the specific capacity of material remains at more than 730mAh/g, also, the material exists
After carrying out multiple charge and discharge under high current density 100mA/g, the reversible capacity of more than 740mAh/g is still maintained.
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