CN108110231B - Carbon-coated Fe4N nano composite material, preparation method and application thereof - Google Patents
Carbon-coated Fe4N nano composite material, preparation method and application thereof Download PDFInfo
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Abstract
The invention provides carbon-coated Fe for a lithium ion negative electrode material4N nano composite material, preparation method and application thereof. The carbon-coated Fe4The size of the N nano composite material is 30-100nm, and the thickness of the carbon coating layer is 5-10 nm. The method comprises the following steps: dicyandiamide is mixed with FeCl3·6H2Dissolving O to obtain a uniformly mixed solution, heating and evaporating to remove water to obtain dicyandiamide and FeCl3·6H2Heating the mixture of O in a tube furnace for reaction, and cooling to obtain Fe4N powder of Fe coated with glucose4N powder, carbonizing to obtain Fe coated with carbon4N nanocomposite electrode materials. The method has the advantages of low preparation cost and simple process, and the prepared carbon-coated Fe4The N nano composite material has uniform appearance, is used for a lithium ion negative electrode material, and has good lithium storage performance, cycle life and rate capability.
Description
Technical Field
The invention relates to the technical field of new energy materials, in particular to carbon-coated Fe for a lithium ion battery cathode material4N nano composite material, preparation method and application in lithium ion battery cathode material.
Background
Lithium ion batteries have been widely used in the fields of energy storage for mobile electronic devices due to their characteristics of high energy, high power density, high safety, environmental friendliness, and the like. Currently, research on lithium ion batteries is progressing towards power battery materials with high energy or power density, good low temperature performance, and high rate performance. The conventional lithium ion battery cathode material is mainly a carbon cathode material, but due to the defects that the theoretical capacity of a commercial graphite cathode is low (372mAh/g), the rate performance is poor, an S EI film (solid electrolyte film) formed in the first charge and discharge greatly causes capacity loss, safety problems are easily caused, and the like, the application of the lithium ion battery cathode material in the field of high-power-density power batteries is greatly limited. In order to develop a high-energy-density and high-safety lithium ion battery cathode material to meet the requirements of a high-power battery and realize higher economic effect and social benefitAnd the deployment of national development strategy, the substitute of the graphite cathode material is urgently needed to be found. The search for new electrode materials is crucial to the development of rechargeable lithium ion batteries with high capacity and excellent stability. The current graphite cathode material substitutes comprise modified graphite, Si-based material, Sn-based material and MnXmType (M is a transition metal and X is a non-metal including O, S, N, P, B or a polymer) material. For MnXmThe lithium storage mechanism of the type material is the partially or completely reversible decomposition of the active material into M0And corresponding lithium salts, which may be simply represented as
The transition metal nitride is expected to be applied to a power battery cathode material due to excellent electrochemical performance and high chemical stability. The particular electronic structure of the transition elements (groups IIIB-VIII) is characterized by the fact that valence electrons can occupy partially filled d orbitals, since electrons are close in energy level between 4s and 3d, 5s and 4d or 6s and 5 d. When the nitride participates in the redox reaction, a multivalent state is generated to efficiently store energy. However, to date, nitrides as active materials have remained far from practical applications because their large volume expansion leads to a rapid capacity fade during the cycling electrochemical reaction.
Disclosure of Invention
In order to solve the above problems, the present invention provides a carbon-coated Fe4N nano composite material, preparation method and application in lithium ion battery cathode material. By mixing Fe4The size of N active material is reduced to nanometer level, the diffusion path and storage time of lithium ion are shortened, the mechanical stress is effectively reduced to adapt to the change of different volumes and improve the cycle capability of electrode material, and Fe is added4The N active material and carbon are compounded to form a carbon coating structure to prevent the carbon coating structure from reacting with electrolyte and protect active substance Fe4N, of increasing materialStability while suppressing the volume expansion effect and Fe4N is easy to agglomerate and the like, carbon has the effect of buffering the excessive volume change of the active substance in the process of cyclic lithium intercalation/lithium deintercalation, the carbon material has certain contribution to the improvement of the battery capacity due to the self lithium ion storage capacity, the carbon compounding improves the conductivity of the electrode and is beneficial to transferring electrons generated in the redox reaction process of the active material to a current collector, and thus, the cycle performance and the rate capability when the carbon is used as the negative electrode material of the lithium ion battery are improved.
The invention adopts the following technical scheme:
carbon-coated Fe4N nanocomposite of said Fe4The surface of the N particle is provided with a carbon coating layer, the thickness of the carbon coating layer is 5-10nm, and the carbon coating layer is Fe4The size of the N nano composite material is 30-100 nm.
Carbon-coated Fe4A method for preparing an N nanocomposite, the method comprising the steps of:
(1) dicyandiamide is mixed with FeCl3·6H2Dissolving O in deionized water, stirring with magnetic stirrer to obtain uniformly mixed solution
(2) Heating the solution obtained in the step (1) until the water in the solution is completely evaporated to dryness to obtain dicyandiamide and FeCl3·6H2A mixture of O;
(3) placing the mixture obtained in the step (2) in a porcelain boat, placing in a tube furnace, and heating to 850-950 ℃ under the argon atmosphere;
(4) when the temperature in the reaction tube in the tube furnace reaches 850-950 ℃, closing argon, introducing ammonia gas into the reaction tube, continuously raising the temperature in the reaction tube to 950-1050 ℃, keeping the temperature for 1-2 hours, continuously introducing ammonia gas until the temperature in the tube furnace is reduced to room temperature, and collecting brown powder on the porcelain boat to obtain Fe4N; wherein the flow rate of the ammonia gas is 80-120 mL/min;
(5) fe obtained in the step (4)4N powder with glucose in a ratio of 1: (1-8) in deionized water, mechanically stirring for 3-5 hours, transferring the final solution to a polytetrafluoroethylene inner container reaction kettle, and placing the reaction kettle in a reaction kettle with a polytetrafluoroethylene inner containerKeeping the temperature in a drying oven at 160-200 ℃ for 8-12 hours, and obtaining glucose coated Fe through centrifugal separation and drying4N powder;
(6) putting the powder obtained in the step (5) into a tube furnace, heating and carbonizing the powder in an argon atmosphere to finally obtain the carbon-coated Fe4An N nanocomposite.
Preferably, in step (1), dicyandiamide and FeCl3·6H2The mass ratio of O to deionized water is (5-10): (3-5): (250-350). Preferably, in step (3), the flow rate of argon is 60-100 mL/min.
Preferably, in step (3), the temperature is raised to 900 ℃ under an argon atmosphere.
Preferably, in step (4), the temperature in the reaction tube is further raised to 1000 ℃ for 1.5 hours.
Preferably, in step (5), the incubation is carried out at 180 ℃ for 10 hours.
Preferably, in the step (6), the carbonization is performed in a tube furnace by raising the temperature to 500 to 900 ℃ for 1 to 2 hours under an argon atmosphere, and more preferably, the carbonization time is 800 ℃ for 1 hour.
The carbon-coated Fe prepared by the invention4N nanocomposite, Fe4The surface of the N nano-particle is provided with a carbon coating layer, the thickness of the carbon coating layer is 5-10nm, and the carbon coating layer is Fe4The size of the N nano composite material is 30-100 nm.
The carbon-coated Fe of the invention4The N nano composite material is used for the lithium ion battery cathode material, and the electrical property cycle test shows that the N nano composite material has good lithium storage performance, cycle life and rate capability: after the charging and discharging cycle is carried out for 100 times, the specific capacity of the material is still kept above 730 mAh/g; moreover, rate performance tests show that the material still maintains high reversible capacity of more than 740mAh/g after being charged and discharged for many times under the condition of high current density of 100mA/g, and the material has good reversibility after being charged and discharged at high rate.
Compared with the prior art, the invention has the following outstanding beneficial effects:
(1) the invention prepares carbon-coated Fe by a hydrothermal method and a high-temperature pyrolysis method4N composite sodiumThe rice material has low production and preparation cost, simple process and easy control;
(2) the carbon-coated Fe prepared by the invention4The N nano composite material has uniform appearance and Fe4The surface of the N nano-particle is provided with a carbon coating layer, the thickness of the carbon coating layer is 5-10nm, and the carbon coating layer is Fe4The size of the N nano composite material is 30-100nm, the active material is reduced to the nano level, the diffusion path and the storage time of lithium ions are shortened, the mechanical stress is effectively reduced to adapt to the changes of different volumes, and the cycle capacity of the electrode material is obviously improved;
(3) the invention is prepared by mixing Fe4The N active material and carbon are compounded to form a carbon coating structure to prevent the carbon coating structure from reacting with electrolyte and protect active substance Fe4N, improving the stability of the material, and simultaneously inhibiting the volume expansion effect and Fe4N is easy to agglomerate and the like;
(4) the carbon-coated Fe prepared by the invention4The N nano composite material used for the lithium ion negative electrode material has good lithium storage performance, cycle life and rate capability, and an electrical performance cycle test shows that: after the charging and discharging are cycled for 100 times, the specific capacity is still kept above 730 mAh/g; and rate performance tests show that the material still maintains the reversible capacity of more than 740mAh/g after being charged and discharged for many times under high current density, namely the reversibility of the material is good after high rate charging and discharging.
Drawings
FIG. 1 is Fe4XRD pattern of N material;
FIG. 2 shows the carbon-coated Fe of the present invention4TEM image of N composite nanomaterial, and (a) and (b) are respectively carbon-coated Fe4Low power and high resolution projection images of N composite nanomaterials;
FIG. 3 shows the carbon-coated Fe of the present invention4A cycle performance diagram of the N composite nano material as a lithium ion battery cathode material;
FIG. 4 shows the carbon-coated Fe of the present invention4And the multiplying power performance diagram of the N composite nano material as the lithium ion battery cathode material.
Detailed Description
Example 1:
(1) dicyandiamide is mixed with FeCl3·6H2Dissolving O in deionized water, and stirring with a magnetic stirrer for 4h to obtain a uniformly mixed solution, wherein dicyandiamide and FeCl3·6H2The mass ratio of O to deionized water is 5: 3: 250 of (a);
(2) heating the solution obtained in the step (1) until the water in the solution is completely evaporated to dryness to obtain dicyandiamide and FeCl3·6H2A mixture of O;
(3) placing the mixture obtained in the step (2) in a porcelain boat, placing in a tube furnace, and heating to 850 ℃ under the argon atmosphere with the flow rate of 60 mL/min;
(4) when the temperature in the reaction tube in the tube furnace reaches 850 ℃, closing argon, introducing 80mL/min ammonia gas into the reaction tube, continuously increasing the temperature in the reaction tube to 950 ℃, continuously introducing the ammonia gas with the flow rate of 80mL/min for 2 hours until the temperature in the tube furnace is reduced to room temperature, and collecting brown powder on the porcelain boat to obtain Fe4N；
(5) Fe obtained in the step (4)4N and glucose were mixed according to a 1: dissolving the solution with the mass ratio of 1 in deionized water, mechanically stirring for 3 hours, transferring the final solution to a polytetrafluoroethylene inner container reaction kettle, placing the reaction kettle in a drying box, preserving the heat at 160 ℃ for 12 hours, and obtaining glucose-coated Fe through centrifugal separation and drying4N powder;
(6) putting the powder obtained in the step (5) into a tube furnace, heating to 500 ℃ in an argon atmosphere, maintaining for 2 hours, and carbonizing to finally obtain carbon-coated Fe4N composite material.
Example 2:
(1) dicyandiamide is mixed with FeCl3·6H2Dissolving O in deionized water, and stirring with a magnetic stirrer for 4h to obtain a uniformly mixed solution, wherein dicyandiamide and FeCl3·6H2The mass ratio of O to deionized water is 6: 4: 280 parts of;
(2) heating the solution obtained in the step (1) until the water in the solution is completely evaporated to dryness,
to obtain dicyandiamide and FeCl3·6H2A mixture of O;
(3) placing the mixture obtained in the step (2) in a porcelain boat, placing in a tube furnace, and heating to 900 ℃ under the argon atmosphere with the flow rate of 80 mL/min;
(4) when the temperature inside the reaction tube in the tube furnace reaches 900 ℃, closing the argon, introducing 100mL/min ammonia gas into the reaction tube, continuously raising the temperature in the reaction tube to 1000 ℃, continuously introducing the ammonia gas with the flow rate of 100mL/min for 1.5 hours until the temperature in the tube furnace is reduced to room temperature, and collecting brown powder on the porcelain boat to obtain Fe4N；
(5) Fe obtained in the step (4)4N and glucose were mixed according to a 1: 2 in deionized water, mechanically stirring for 4 hours, transferring the final solution to a polytetrafluoroethylene inner container reaction kettle, placing the reaction kettle in a drying box, preserving the heat at 180 ℃ for 10 hours, and obtaining the glucose-coated Fe through centrifugal separation and drying4N powder;
(6) putting the powder obtained in the step (5) into a tube furnace, heating to 600 ℃ in an argon atmosphere, maintaining for 1 hour for carbonization, and finally obtaining carbon-coated Fe4N composite material.
Example 3:
(1) dicyandiamide is mixed with FeCl3·6H2Dissolving O in deionized water, stirring for 4h with a magnetic stirrer,
obtaining a uniformly mixed solution of dicyandiamide and FeCl3·6H2The mass ratio of O to deionized water is 8: 5: 300, respectively;
(2) heating the solution obtained in the step (1) until the water in the solution is completely evaporated to dryness,
to obtain dicyandiamide and FeCl3·6H2A mixture of O;
(3) placing the mixture obtained in the step (2) in a porcelain boat, placing in a tube furnace, and heating to 950 ℃ under the argon atmosphere with the flow rate of 100 mL/min;
(4) when the temperature in the reaction tube in the tube furnace reaches 950 ℃, closing the argon, introducing 120mL/min ammonia gas into the reaction tube, continuously increasing the temperature in the reaction tube to 1050 ℃, and continuing for 1 hourContinuously introducing ammonia gas with the flow rate still being 120mL/min until the temperature of the tube furnace is reduced to the room temperature, and collecting brown powder on the porcelain boat to obtain Fe4N；
(5) Fe obtained in the step (4)4N and glucose were mixed according to a 1: 4 in deionized water, mechanically stirring for 5 hours, transferring the final solution to a polytetrafluoroethylene inner container reaction kettle, placing the reaction kettle in a drying box, preserving the heat at 200 ℃ for 8 hours, and obtaining the glucose-coated Fe through centrifugal separation and drying4N powder;
(6) putting the powder obtained in the step (5) into a tube furnace, heating to 800 ℃ in an argon atmosphere, maintaining for 1 hour for carbonization, and finally obtaining carbon-coated Fe4N composite material.
Example 4:
(1) dicyandiamide is mixed with FeCl3·6H2Dissolving O in deionized water, and stirring with a magnetic stirrer for 4h to obtain a uniformly mixed solution, wherein dicyandiamide and FeCl3·6H2The mass ratio of O to deionized water is 10: 5: 350 of (a);
(2) heating the solution obtained in the step (1) until the water in the solution is completely evaporated to dryness to obtain dicyandiamide and FeCl3·6H2A mixture of O;
(3) placing the mixture obtained in the step (2) in a porcelain boat, placing in a tube furnace, and heating to 900 ℃ under the argon atmosphere with the flow rate of 80 mL/min;
(4) when the temperature inside the reaction tube in the tube furnace reaches 900 ℃, closing the argon, introducing 100mL/min ammonia gas into the reaction tube, continuously raising the temperature in the reaction tube to 1000 ℃, continuously introducing the ammonia gas with the flow rate of 100mL/min for 1.5 hours until the temperature in the tube furnace is reduced to room temperature, and collecting brown powder on the porcelain boat to obtain Fe4N；
(5) Fe obtained in the step (4)4N and glucose were mixed according to a 1: 8 in deionized water, mechanically stirring for 4 hours, transferring the final solution to a polytetrafluoroethylene inner container reaction kettle, placing the reaction kettle in a drying box, preserving the heat at 180 ℃ for 10 hours, and obtaining the glucose coated Fe through centrifugal separation and drying4N powder;
(6) putting the powder obtained in the step (5) into a tube furnace, heating to 900 ℃ in an argon atmosphere, maintaining for 1 hour for carbonization, and finally obtaining carbon-coated Fe4N composite material.
Further, the carbon-coated Fe prepared by the embodiment of the invention4TEM observation analysis is carried out on the N composite material, wherein FIG. 2(a) and FIG. 2(b) are respectively carbon-coated Fe4The low-power and high-resolution projection images of the N composite nano material show that the carbon-coated Fe prepared by the invention4The N composite material is of a nano structure with uniform appearance and Fe4The surface of the N nano-particle is provided with a carbon coating layer, the thickness of the carbon coating layer is 5-10nm, and the carbon coating layer is Fe4The size of the N nano composite material is 30-100 nm.
Furthermore, the carbon-coated Fe prepared by the embodiment of the invention4The N nano composite material is used for a lithium ion battery cathode material, an electrical property cycle test is carried out, the test result is shown in a cycle performance diagram shown in figure 3 and a rate performance diagram shown in figure 4, and the N nano composite material has good lithium storage performance, cycle life and rate performance: after charging and discharging for 100 times, the specific capacity is still kept above 730mAh/g, the reversible capacities of the material disclosed by the invention shown in the figure 4 after multiple charging and discharging are 766mAh/g, 665mAh/g, 475mAh/g, 250mAh/g and 746mAh/g respectively under the condition that different current densities are 100mA/g, 200mA/g, 500mA/g, 1000mA/g and 100mA/g, so that the material still keeps higher reversible capacity after multiple charging and discharging under high current density, namely the material still keeps higher reversible capacity during high-rate charging and discharging, and the reversibility of the material is good.
The above-described embodiments of the present invention should not be construed as limiting the scope of the present invention. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (7)
1. A method for preparing a carbon-coated Fe4N nanocomposite for a lithium ion battery anode material is characterized by comprising the following steps: fe4The surface of the N particle is provided with a carbon coating layer, the thickness of the carbon coating layer is 5-10nm, and the carbon coating layer is Fe4The size of the N nano composite material is 30-100 nm; the method comprises the following steps:
(1) dissolving dicyandiamide and FeCl3 & 6H2O in deionized water, and stirring by using a magnetic stirrer to obtain a uniformly mixed solution;
(2) heating the solution obtained in the step (1) until the water in the solution is completely evaporated to dryness to obtain a mixture of dicyandiamide and FeCl3 & 6H 2O;
(3) placing the mixture obtained in the step (2) in a porcelain boat, placing in a tube furnace, and heating to 850-950 ℃ under the argon atmosphere;
(4) when the temperature in the reaction tube in the tube furnace reaches 850-950 ℃, closing argon, introducing ammonia gas into the reaction tube, continuously raising the temperature in the reaction tube to 950-1050 ℃, keeping the temperature for 1-2 hours, continuously introducing ammonia gas until the temperature in the tube furnace is reduced to room temperature, and collecting brown powder on the porcelain boat to obtain Fe 4N; wherein the flow rate of the ammonia gas is 80-120 mL/min;
(5) mixing the Fe4N powder obtained in the step (4) with glucose according to the ratio of 1: (1-8) dissolving the mass ratio in deionized water, mechanically stirring for 3-5 hours, transferring the final solution into a polytetrafluoroethylene liner reaction kettle, placing the reaction kettle in a drying box, keeping the temperature at 160-200 ℃ for 8-12 hours, and performing centrifugal separation and drying to obtain powder of glucose-coated Fe 4N;
(6) and (5) putting the powder obtained in the step (5) into a tubular furnace, and heating and carbonizing the powder in an argon atmosphere to finally obtain the carbon-coated Fe4N nano composite material.
2. The method of claim 1, wherein: in the step (1), the mass ratio of dicyandiamide to FeCl3 & 6H2O to deionized water is (5-10): (3-5): (250-350).
3. The method according to claim 1 or 2, characterized in that: in the step (3), the flow rate of argon gas is 60-100 mL/min, and the temperature is increased to 900 ℃ under the argon atmosphere.
4. The method according to claim 1 or 2, characterized in that: in step (4), the temperature in the reaction tube was further raised to 1000 ℃ and maintained for 1.5 hours.
5. The method according to claim 1 or 2, characterized in that: in the step (5), the mixture is placed in a drying oven and is kept at 180 ℃ for 10 hours.
6. The method according to claim 1 or 2, characterized in that: in the step (6), the temperature is increased to 500-900 ℃ and maintained for 1-2 hours for carbonization.
7. The method according to claim 6, wherein in the step (6), the carbonization is performed by raising the temperature to 800 ℃ for 1 hour.
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| CN109742350B (en) * | 2018-12-28 | 2021-11-19 | 上海应用技术大学 | Preparation method of nitrided ferroferric oxide/graphene composite material |
| CN111883754A (en) * | 2020-07-21 | 2020-11-03 | 合肥国轩高科动力能源有限公司 | Iron nitride-ordered mesoporous carbon composite material and preparation method and application thereof |
| CN113980464B (en) * | 2021-11-23 | 2024-05-07 | 深圳市北测检测技术有限公司 | Based on Fe4N preparation of Fe4Method for preparing N@PANI nano composite wave-absorbing material |
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