CN113113584B - NiFe-LDH composite C3N4@Mo2Preparation method of C battery electrode material - Google Patents
NiFe-LDH composite C3N4@Mo2Preparation method of C battery electrode material Download PDFInfo
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Abstract
The invention discloses a NiFe-LDH composite C3N4@Mo2The preparation method of the C battery electrode material comprises the steps of firstly, utilizing melamine as a raw material, and calcining to obtain C3N4Then taking the mixture of ammonium molybdate and urea-formaldehyde resin as a reaction solution and C3N4Preparing C by using a rapid cooling mode for the core3N4@Mo2C, a core-shell structure; on the basis, synthesis of LDH and C are realized under hydrothermal conditions by the traditional LDH preparation method3N4@Mo2And C, synchronously compounding a core-shell structure. The invention will C3N4@Mo2The C core-shell structure is loaded in the NiFe-LDH material, and the characteristics of large specific surface area and large loading density of the LDH material are utilized to fully exert the LDH material and Mo2The advantages of the two, the obtained battery electrode material NiFe-LDH composite C3N4@Mo2The C has high coulombic efficiency and capacity and excellent cycling stability, and is an electrode material with good development prospect.
Description
Technical Field
The invention relates to a preparation method of a composite material, in particular to NiFe-LDH composite C3N4@Mo2And C, a preparation method of the battery electrode material.
Background
Layered Double Hydroxides (LDHs) are a general term for Hydrotalcite (HT) and Hydrotalcite-Like Compounds (HTLCs).
LDH has large specific surface area and good performances such as load and catalysis, and is a great research hotspot in the field of electrode materials. For example, chinese patent application CN106601500A discloses a modification method of NiFe-LDH electrode material, which effectively improves the problems of hydrogen evolution, etc., but introduces new impurities during the preparation process, which affects the cycling stability of the electrode material.
Recently, professor Chengchun issued a paper entitled "free and imaging and/or N-lateral carbon foam as effective polymeric foam and catalyst for high performance carbon foams" and disclosed a molybdenum carbide-graphene-nitrogen doped carbon foam (GCF-G @ Mo) with three-dimensional hierarchical structure2C) The composite material is compounded with sulfur to form the positive electrode material of the lithium-sulfur battery. It is noted that the composite material has the following advantages: (1) in the electrode, the graphene is wrapped on the framework of melamine carbon foam and has layersThe porous structure is organized, which can suppress the shuttling effect of polysulfides by physical confinement. 2) Graphitized carbon foam resulting from the carbonization of melamine foam has a high nitrogen content (6.17 at%), which can further inhibit the shuttling of polysulfides by chemisorption. (3) Metallic molybdenum carbide (Mo)2C) The nano particles have good conductivity and excellent catalytic effect, can promote the rapid transfer of electrons, play the role of a polar fixing agent and a catalyst, and provide more active sites for the efficient catalytic conversion of polysulfide. It can be seen that the presence of the metal molybdenum carbide has a positive promoting effect on improving the performance of the electrode material.
Disclosure of Invention
On the basis of the research, the invention provides a NiFe-LDH composite C for further improving the coulombic efficiency, the battery capacity and the cycling stability of a battery electrode material3N4@Mo2The preparation method of the battery electrode material comprises the following specific steps:
s1: melamine is taken as a raw material, placed in a ceramic crucible, covered with a crucible cover, and calcined in a muffle furnace to obtain C3N4；
S2: preparing ammonium molybdate into a solution with the concentration of 1.2-2mol/L, wherein the solvent is a mixed solvent of deionized water and ethanol with the volume ratio of (4-6) to 1, then heating to 60 ℃, and adding uncured urea-formaldehyde resin during stirring to obtain a reaction solution;
s3: adding C obtained in step 1 to the reaction solution obtained in S23N4Slowly stirring, heating to slightly boil the mixed liquid, rapidly transferring to ethylene glycol aqueous solution at-6 deg.C, rapidly cooling for 30s-1min, filtering, and washing with deionized water to obtain C3N4@Mo2C, core-shell structure products;
s4: dissolving nickel nitrate and ferric nitrate into deionized water according to the molar ratio of 1: 1, adding urea and CTAB, stirring for 20-30min, transferring the mixed solution into a polytetrafluoroethylene reaction kettle, and adding C obtained from S3 under stirring3N4@Mo2C core-shell structure product, performing hydrothermal treatment at 130-160 DEG CAfter the reaction, washing the product with deionized water, and drying for 1h in an inert gas environment at constant temperature to obtain the NiFe-LDH composite C3N4@Mo2C, battery electrode material.
Preferably, in the step S1, the addition amount of melamine is 85-90% of the volume of the ceramic crucible.
Preferably, in the step S1, the calcination condition is to heat up to 550 ℃ and 560 ℃ at a heating rate of 5-6 ℃/min, and the temperature is maintained for 3 h.
Preferably, in step S2, the molar ratio of ammonium molybdate to urea-formaldehyde resin is 1: 4-7, wherein the uncured urea-formaldehyde resin refers to an initial urea-formaldehyde resin formed by condensation polymerization of urea and formaldehyde under the action of a catalyst.
Preferably, in step S3, C3N4In a molar ratio of 1: 3-5 with the ammonium molybdate in the S2.
Preferably, in the step S4, the concentration of nickel nitrate is controlled to be 0.6-1mol/L, the concentration of urea is controlled to be 2-6mol/L, and the concentration of CTAB is controlled to be 0.06-0.1 mol/L.
Preferably, in step S4, C3N4@Mo2The molar ratio of the C core-shell structure product to the nickel nitrate is 0.1-0.8: 1.
Preferably, in the step S4, the hydrothermal reaction time is 1.5-4h, and the constant temperature drying temperature is 70-90 ℃.
In the invention, firstly, melamine is used as a raw material and calcined to obtain C3N4Then taking the mixture of ammonium molybdate and urea-formaldehyde resin as a reaction solution and C3N4Preparing C for nucleus by quick cooling3N4@Mo2C, a core-shell structure; on the basis, synthesis of LDH and C are realized under hydrothermal conditions by the traditional LDH preparation method3N4@Mo2And C, synchronously compounding a core-shell structure.
The invention utilizes urea formaldehyde resin as a carbon source to react with ammonium molybdate quickly in the boiling-extremely cold process, and can form uniform coating C3N4Shell structure Mo of surface2C, the material C is a composite material,and the obtained product particles are ensured to be fine and uniform by a rapid cooling mode. C of graphite-like phase3N4As core structure, it provides sufficient ion transmission channel for battery electrode material to work, and Mo of shell structure2C promotes the rapid transfer of electrons.
The invention synthesizes LDH material and simultaneously leads C to react by hydrothermal reaction3N4@Mo2The C core-shell structure is loaded in the NiFe-LDH material, and the characteristics of large specific surface area and large loading density of the LDH material are utilized to fully exert the LDH material and Mo2The advantages of the C, and the obtained battery electrode material NiFe-LDH composite C3N4@Mo2The C has high coulombic efficiency and capacity and excellent cycling stability, and is a battery electrode material with good development prospect.
Detailed Description
In order to better explain the present invention, the invention is explained and illustrated by the following detailed description.
Example 1
NiFe-LDH composite C3N4@Mo2The preparation method of the electrode material of the C battery comprises the following steps:
s1: putting melamine serving as a raw material into a ceramic crucible, wherein the addition amount of the melamine is 85% of the volume of the ceramic crucible, covering a crucible cover, heating to 550 ℃ in a muffle furnace at a heating rate of 6 ℃/min, and preserving heat for 3h to obtain C3N4；
S2: preparing ammonium molybdate into a solution with the concentration of 2mol/L, wherein the solvent is a mixed solvent of deionized water and ethanol with the volume ratio of 4: 1, then heating to 60 ℃, adding uncured urea-formaldehyde resin according to the molar ratio of 1: 4 of ammonium molybdate to urea-formaldehyde resin in the stirring process, and stirring to obtain a reaction solution;
s3: adding C obtained in step 1 to the reaction solution obtained in S23N4Slowly stirring, heating to slightly boil the mixed liquid, quickly transferring to ethylene glycol aqueous solution at-6 deg.C, quenching and holding for about 30s, filtering the product, and washing with deionized water to obtain the final productTo C3N4@Mo2A core-shell structure product of C, wherein C3N4In a molar ratio of 1: 3 with the ammonium molybdate in the S2;
s4: dissolving nickel nitrate and ferric nitrate into deionized water according to the molar ratio of 1: 1, adding urea and CTAB, stirring for 20min to obtain a mixed solution, wherein the concentration of nickel nitrate is 1mol/L, the concentration of urea is 2mol/L, and the concentration of CTAB is 0.1mol/L, transferring the mixed solution into a polytetrafluoroethylene reaction kettle, and adding C obtained from S3 under the stirring state3N4@Mo2Carrying out hydrothermal reaction on the C core-shell structure product at 130 ℃ for 3h, cleaning the product with deionized water after the reaction is finished, and drying the product at the constant temperature of 70 ℃ for 1h in an inert gas environment to obtain the NiFe-LDH composite C3N4@Mo2C cell electrode material, wherein C3N4@Mo2The molar ratio of the C core-shell structure product to the nickel nitrate is 0.3: 1.
The composite material obtained in example 1 and sulfur composite were used as a positive electrode material of a lithium-sulfur battery, and the battery was assembled to test electrical properties: at a current density of 1C, the capacity was 1033mAh/g, and the capacity drop was 4.72% and 14.93% under the condition of the cycle test, 100 cycles and 300 cycles. Therefore, the composite material prepared by the invention has good electrical property and cycling stability when being used as a battery electrode material,
example 2
NiFe-LDH composite C3N4@Mo2The preparation method of the electrode material of the C battery comprises the following steps:
s1: putting melamine serving as a raw material into a ceramic crucible, covering a crucible cover, heating to 560 ℃ in a muffle furnace at a heating rate of 5 ℃/min, and preserving heat for 3h to obtain C3N4；
S2: preparing ammonium molybdate into a solution with the concentration of 1.2mol/L, wherein the solvent is a mixed solvent of deionized water and ethanol with the volume ratio of 6: 1, then heating to 60 ℃, adding uncured urea-formaldehyde resin according to the molar ratio of 1: 7 of ammonium molybdate to urea-formaldehyde resin in the stirring process, and stirring to obtain a reaction solution;
s3: adding C obtained in step 1 to the reaction solution obtained in S23N4Slowly stirring, heating to slightly boil the mixed liquid, rapidly transferring to ethylene glycol aqueous solution at-6 deg.C, rapidly cooling, maintaining for about 1min, filtering, and washing with deionized water to obtain C3N4@Mo2A core-shell structure product of C, wherein C3N4In a molar ratio of 1: 5 with the ammonium molybdate in the S2;
s4: dissolving nickel nitrate and ferric nitrate into deionized water according to the molar ratio of 1: 1, adding urea and CTAB, stirring for 30min to obtain a mixed solution, wherein the concentration of nickel nitrate is 0.6mol/L, the concentration of urea is 4mol/L, and the concentration of CTAB is 0.06mol/L, transferring the mixed solution into a polytetrafluoroethylene reaction kettle, and adding C obtained from S3 under stirring3N4@Mo2Carrying out hydrothermal reaction on the C core-shell structure product at 160 ℃ for 1.5h, cleaning the product with deionized water after the reaction is finished, and drying the product at the constant temperature of 90 ℃ for 1h in an inert gas environment to obtain the NiFe-LDH composite C3N4@Mo2C cell electrode material, wherein C3N4@Mo2The molar ratio of the C core-shell structure product to the nickel nitrate is 0.8: 1.
Example 3
NiFe-LDH composite C3N4@Mo2The preparation method of the electrode material of the C battery comprises the following steps:
s1: putting melamine serving as a raw material into a ceramic crucible, wherein the addition amount of the melamine is 90 percent of the volume of the ceramic crucible, covering a crucible cover, heating to 550 ℃ in a muffle furnace at a heating rate of 5 ℃/min, and preserving heat for 3h to obtain C3N4；
S2: preparing ammonium molybdate into a solution with the concentration of 1.5mol/L, wherein the solvent is a mixed solvent of deionized water and ethanol with the volume ratio of 5: 1, then heating to 60 ℃, adding uncured urea-formaldehyde resin according to the molar ratio of 1: 5 of ammonium molybdate to urea-formaldehyde resin in the stirring process, and stirring to obtain a reaction solution;
s3: adding C obtained in step 1 to the reaction solution obtained in S23N4Slowly stirring, heating to slightly boil the mixed liquid, quickly transferring to ethylene glycol aqueous solution at-6 deg.C, quenching and holding for about 40s, filtering the product, and washing with deionized water to obtain C3N4@Mo2A core-shell structure product of C, wherein C3N4In a molar ratio of 1: 7 with the ammonium molybdate in the S2;
s4: dissolving nickel nitrate and ferric nitrate into deionized water according to the molar ratio of 1: 1, adding urea and CTAB, stirring for 20min to obtain a mixed solution, wherein the concentration of nickel nitrate is 0.75mol/L, the concentration of urea is 5.5mol/L, and the concentration of CTAB is 0.07mol/L, transferring the mixed solution into a polytetrafluoroethylene reaction kettle, and adding C obtained from S3 under stirring3N4@Mo2Carrying out hydrothermal reaction on the C core-shell structure product at 140 ℃ for 4h, cleaning the product with deionized water after the reaction is finished, and drying the product at the constant temperature of 90 ℃ for 1h in an inert gas environment to obtain the NiFe-LDH composite C3N4@Mo2C cell electrode material, wherein C3N4@Mo2The molar ratio of the C core-shell structure product to the nickel nitrate is 0.65: 1.
Claims (8)
1. NiFe-LDH composite C3N4@Mo2The preparation method of the electrode material of the C battery is characterized by comprising the following steps:
s1: melamine is used as a raw material, placed in a ceramic crucible, covered with a crucible cover, and calcined in a muffle furnace to obtain C3N4；
S2: preparing ammonium molybdate into a solution with the concentration of 1.2-2mol/L, wherein the solvent is a mixed solvent of deionized water and ethanol with the volume ratio of (4-6) to 1, then heating to 60 ℃, and adding uncured urea-formaldehyde resin during stirring to obtain a reaction solution;
s3: adding C obtained in step S1 to the reaction solution obtained in step S23N4Slowly stirring, heating to slightly boiling, and quickly moving to-6 deg.CQuenching in alcohol-water solution for 30s-1min, filtering, washing with deionized water to obtain C3N4@Mo2C, core-shell structure products;
s4: dissolving nickel nitrate and ferric nitrate into deionized water according to the molar ratio of 1: 1, adding urea and CTAB, stirring for 20-30min, transferring the mixed solution into a polytetrafluoroethylene reaction kettle, and adding C obtained from S3 under stirring3N4@Mo2Performing hydrothermal reaction on the C core-shell structure product at the temperature of 130-160 ℃, cleaning the product with deionized water after the reaction is finished, and drying the product for 1h at constant temperature in an inert gas environment to obtain the NiFe-LDH composite C3N4@Mo2And C, material.
2. A NiFe-LDH complex C of claim 13N4@Mo2The preparation method of the C battery electrode material is characterized in that in the step S1, the addition amount of melamine is 85-90% of the volume of the ceramic crucible.
3. A NiFe-LDH composite C of claim 13N4@Mo2The preparation method of the battery electrode material is characterized in that in the step S1, the calcining condition is that the temperature is raised to 550-560 ℃ at the temperature raising rate of 5-6 ℃/min, and the temperature is kept for 3 h.
4. A NiFe-LDH complex C of claim 13N4@Mo2The preparation method of the battery electrode material C is characterized in that in the step S2, the molar ratio of ammonium molybdate to urea-formaldehyde resin is 1: 4-7.
5. A NiFe-LDH complex C of claim 13N4@Mo2The preparation method of the C battery electrode material is characterized in that in the step S3, C3N4In a molar ratio of 1: 3-5 to the ammonium molybdate in said step S2.
6. The method of claim 1NiFe-LDH composite C3N4@Mo2The preparation method of the battery electrode material is characterized in that in the step S4, the concentration of nickel nitrate is controlled to be 0.6-1mol/L, the concentration of urea is controlled to be 2-6mol/L, and the concentration of CTAB is controlled to be 0.06-0.1 mol/L.
7. A NiFe-LDH complex C of claim 13N4@Mo2The preparation method of the C battery electrode material is characterized in that in the step S4, C3N4@Mo2The molar ratio of the C core-shell structure product to the nickel nitrate is 0.1-0.8: 1.
8. A NiFe-LDH complex C of claim 13N4@Mo2The preparation method of the C battery electrode material is characterized in that in the step S4, the hydrothermal reaction time is 1.5-4h, and the constant-temperature drying temperature is 70-90 ℃.
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| CN106241877A (en) * | 2016-07-15 | 2016-12-21 | 江苏大学 | A kind of g C3n4/ MoS2the preparation method of/ZnS nano composite material |
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