CN106602023B - A kind of method of fabricated in situ graphite phase carbon nitride-oxidation carbon/carbon-copper composite material - Google Patents

A kind of method of fabricated in situ graphite phase carbon nitride-oxidation carbon/carbon-copper composite material Download PDF

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CN106602023B
CN106602023B CN201611219983.3A CN201611219983A CN106602023B CN 106602023 B CN106602023 B CN 106602023B CN 201611219983 A CN201611219983 A CN 201611219983A CN 106602023 B CN106602023 B CN 106602023B
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composite material
cuo
fabricated
situ
solvent
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CN106602023A (en
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李昱
韦方艳
张润霖
刘婧
吴旻
陈丽华
阳晓宇
苏宝连
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Wuhan University of Technology WUT
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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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • 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 invention discloses a kind of fabricated in situ g-C3N4The method of/CuO composite material includes the following steps: 1) to stir evenly acetonitrile and organic solvent, obtains mixed reaction solvent；2) dicyan diamino and copper nitrate stirring and dissolving in the mixed reaction solvent obtained by step 1), are obtained into precursor solution；3) precursor solution is heated and carries out solvent thermal reaction, then carried out separating-purifying drying, obtain g-C3N4/ CuO composite material.Preparation method of the present invention is simple, and reaction condition is mild, and process is simple, the g-C of preparation3N4The storage lithium performance that/CuO composite material has good cycling stability, electrode specific capacity high, can be used as lithium ion battery negative material.

Description

A kind of method of fabricated in situ graphite phase carbon nitride-oxidation carbon/carbon-copper composite material
Technical field
The invention belongs to the exploitation of new energy materials and studying technological domains, and in particular to a kind of fabricated in situ graphite-phase nitrogen Change carbon-oxidation carbon/carbon-copper composite material method and application.
Background technique
Lithium ion battery is as energy conversion device of new generation, due to its high-energy density, invertibity and cycle life The significant advantages such as long are widely studied.In order to meet the requirement of high-energy density and high power density, exploitation has height The negative electrode material of high rate performance and high security, to replace traditional Carbon anode, it has also become a urgent task.Carbon anode by It is seriously limited in its lower theoretical capacity (graphite 372mA h/g), poor lithium ion intercalation dynamics and safety issue The development and application of cell negative electrode material are made.CuO has high lithium storage content, theoretical capacity as ion cathode material lithium It is the 2 times or more of plumbago-carbon negative pole material for 674mA h/g.Currently, the cyclical stability of pure phase CuO negative electrode material is not high, lead to Compound coating is carried out frequently with graphene, conducting polymer and other materials, the electric conductivity and structural stability for improving CuO are come Improve its cycle life.High molecular polymer g-C3N4The theoretical capacity of ion cathode material lithium is 524 (Li2C3N4) and 534 (Li2C4N3) mAh/g, with good electric conductivity and higher theoretical capacity, therefore g-C3N4/ CuO composite material is used for Lithium-ion negative pole has very big research and application value.
The preparation method of composite material can be divided into one-step method and method of fractional steps synthesis.Currently, preparation g-C3N4/ CuO composite wood The method of material is mainly the method for fractional steps.There are the dispersions of the second phase for method of fractional steps synthetic composite material unevenly, and interface cohesion is insecure etc. Problem.Interface free from admixture pollution between the second phase and matrix of one-step synthesis method composite material, there is ideal original position between the two Matching, can significantly improve the bonding state of two-phase interface in material, and material is made to have excellent physical and chemical performance.Currently, one The technical deficiency of footwork synthesis, is difficult to regulate and control nucleation and the growth of a variety of crystal phases simultaneously in the same system, obtain Product is typically only physical mixed, cannot get two-phase or multiphase composite material, greatly reduces the performance of composite material.One step Method fabricated in situ g-C3N4/ CuO composite material has excellent interface fine structure, can be effectively reduced the embedding lithium-of battery charging and discharging Volume change bring adversely affects during de- lithium, and the structure of stabilizing actives improves cycle life.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of fabricated in situ g-C3N4/ CuO composite material Method, simple process that this method is related to, reaction condition are mild, the g-C of preparation3N4/ CuO composite material has stable circulation Property good, storage lithium performance that electrode specific capacity is high, be suitble to promote and apply.
To achieve the goals above, the technical solution adopted by the present invention are as follows:
A kind of fabricated in situ g-C3N4The method of/CuO composite material, includes the following steps:
1) acetonitrile and organic solvent are stirred evenly, obtains mixed reaction solvent；
2) dicyan diamino and copper nitrate stirring and dissolving in the mixed reaction solvent obtained by step 1), are obtained into precursor solution；
3) gained precursor solution is heated and carries out solvent thermal reaction, then carried out separating-purifying drying, obtain g-C3N4/CuO Powder；
4) g-C for obtaining step 3)3N4/ CuO powder, which is placed in Muffle furnace, is heat-treated (annealing) to get height The g-C of crystallinity3N4/ CuO composite material (graphite phase carbon nitride-oxidation carbon/carbon-copper composite material).
In above scheme, the organic solvent is n,N-Dimethylformamide (DMF).
In above scheme, the volume ratio of the acetonitrile and organic solvent is 1:(0.05~5.0).
In above scheme, the molar ratio of the dicyan diamino and copper nitrate is 1:(0.1~1.0).
Preferably, the copper nitrate and the mass ratio of n,N-Dimethylformamide are 1:(3~15).
In above scheme, stirring and dissolving time described in step 1) is 0.5~6h.
In above scheme, the solvent thermal reaction temperature is 150~220 DEG C, and the reaction time is 6~48h.
Preferably, the solvent thermal reaction temperature be 180~200 DEG C, the reaction time be 12~for 24 hours.
In above scheme, the heat treatment temperature is 250~350 DEG C, and the time is 1~4h.
The g-C according to made from above scheme3N4/ CuO composite material, it is in nano wire microballoon, nano particle microballoon or nanometer Piece micro-sphere structure, the micro-sphere structure being respectively made of nano wire, nano particle, nanometer sheet, Microsphere Size are 400~500nm； The ratio or solvent heat temperature, time of change reactant, the microscopic appearance of controlled material can be passed through.
G-C described in above scheme3N4Application of/CuO the composite material in negative electrode of lithium ion battery.
The present invention is anti-with acetonitrile and n,N-Dimethylformamide (DMF) using dicyan diamino and copper nitrate as primary raw material Answer solvent.Acetonitrile promotes dicyan diamino that polycondensation reaction occurs, the amido with the progress of polycondensation reaction, in dicyan diamino strand Disconnected strong abjection occurs, amido and water reaction generate ammonium hydroxide and OH-, make the aobvious alkalinity of solution；N,N-dimethylformamide (DMF) and nitre Complex reaction occurs for sour copper, and control crystal grain is grown up, while and g-C3N4The OH that polycondensation deamination generates-Reaction, first generates Cu (OH)2Precipitating, final reaction generate CuO, and the synergistic effect of the two finally obtains the g-C of In-situ reaction3N4/ CuO composite material, The complex crystallization that solvent heat obtains is lower, and the crystallinity of material is improved by subsequent thermal anneal process.
Compared with prior art, the invention has the benefit that preparation method of the present invention is simple, reaction condition temperature With process simplicity, the g-C of preparation3N4The storage lithium performance that/CuO composite material has good cycling stability, electrode specific capacity high.
Detailed description of the invention
Fig. 1 is X-ray diffraction (XRD) figure of 1 gained final product of the embodiment of the present invention.
Fig. 2 is scanning electron microscope (SEM) figure of 1 gained final product of the embodiment of the present invention.
Fig. 3 is the cycle performance of lithium ion battery figure of 1 gained final product of the embodiment of the present invention.
Fig. 4 is X-ray diffraction (XRD) figure of 2 gained final product of the embodiment of the present invention.
Fig. 5 is scanning electron microscope (SEM) figure of 2 gained final product of the embodiment of the present invention.
Fig. 6 is scanning electron microscope (SEM) figure of 3 gained final product of the embodiment of the present invention.
Fig. 7 is scanning electron microscope (SEM) figure of 4 gained final product of the embodiment of the present invention.
Fig. 8 is scanning electron microscope (SEM) figure of 5 gained final product of the embodiment of the present invention.
Specific embodiment
For a better understanding of the present invention, below with reference to the example content that the present invention is furture elucidated, but the present invention is not only It is limited only to the following examples.
In following embodiment, the reagent used unless specific instructions is commercially available chemical reagent.
Embodiment 1
A kind of fabricated in situ g-C3N4The method of/CuO composite material, includes the following steps:
1) it weighs 40mL acetonitrile and 10mL n,N-Dimethylformamide (DMF) is mixed in 250mL beaker, obtain mixed Close reaction dissolvent；
2) it weighs 1.5g dicyan diamino and 2.155g copper nitrate is dissolved in mixed reaction solvent obtained by step 1) that (magnetic force stirs Mix 2h), obtain precursor solution；
3) precursor solution for obtaining step 2) is transferred in the reaction kettle of 100mL polytetrafluoroethyllining lining and is heated to 200 DEG C of progress solvent thermal reactions for 24 hours, obtain the g-C of black after reaction kettle naturally cools to room temperature3N4/ CuO solution, then first Separating-purifying is filtered with 3~5 deionized waters and 1~3 ethyl alcohol afterwards, finally 12h is dried in 60 DEG C of baking ovens, obtains g-C3N4/CuO Powder；
4) g-C for obtaining step 3)3N4/ CuO powder, which is placed in Muffle furnace, is heated to 300 DEG C of heat treatment 2h, obtains highly crystalline The g-C of degree3N4/ CuO composite material.
The XRD spectrum of final product obtained by the present embodiment is shown in Fig. 1, shows g-C in figure3N4It is obvious with the diffraction maximum of CuO, knot Brilliant degree is high；Fig. 2 is scanning electron microscope (SEM) figure of final product obtained by the present embodiment, shows g-C in figure3N4/ CuO composite material Pattern is uniform, is in 400~500nm nano wire microballoon；Fig. 3 is that the lithium ion battery charge and discharge of final product obtained by the present embodiment follow Ring performance map shows its chemical property high with good cycling stability, electrode specific capacity in figure.
Embodiment 2
A kind of fabricated in situ g-C3N4The method and application of/CuO composite material, include the following steps:
1) 33.3mL acetonitrile and 16.7mLN are weighed, dinethylformamide (DMF) is mixed in 250mL beaker, obtains Mixed reaction solvent；
2) it weighs 1.5g dicyan diamino and 2.155g copper nitrate is dissolved in mixed reaction solvent obtained by step 1) that (magnetic force stirs Mix 2h), obtain precursor solution；
3) precursor solution for obtaining step 2) is transferred in the reaction kettle of 100mL polytetrafluoroethyllining lining and is heated to 200 DEG C of progress solvent thermal reactions for 24 hours, obtain the g-C of black after reaction kettle naturally cools to room temperature3N4/ CuO solution, then first Separating-purifying is filtered with 3~5 deionized waters and 1~3 ethyl alcohol afterwards, finally 12h is dried in 60 DEG C of baking ovens, obtains g-C3N4/CuO Powder；
4) g-C for obtaining step 3)3N4/ CuO powder 300 DEG C of heat treatment 2h in Muffle furnace, obtain the g- of high-crystallinity C3N4/ CuO composite material.
The XRD spectrum of final product obtained by the present embodiment is shown in Fig. 4, shows g-C in figure3N4It is obvious with the diffraction maximum of CuO, knot Crystalline substance is high；Fig. 5 is scanning electron microscope (SEM) figure of final product obtained by the present embodiment, shows g-C in figure3N4/ CuO composite material shape Looks are uniform, are in 400~500nm nanometer sheet microballoon.
Embodiment 3
A kind of fabricated in situ g-C3N4The method and application of/CuO composite material, include the following steps:
1) 40mL acetonitrile and 10mLN are weighed, dinethylformamide (DMF) is mixed in 250mL beaker, must mix Reaction dissolvent；
2) it weighs 1.5g dicyan diamino and 2.155g copper nitrate is dissolved in mixed reaction solvent obtained by step 1) that (magnetic force stirs Mix 2h), obtain precursor solution；
3) precursor solution for obtaining step 2) is transferred in the reaction kettle of 100mL polytetrafluoroethyllining lining and is heated to 150 DEG C of progress solvent thermal reactions for 24 hours, obtain the g-C of black after reaction kettle naturally cools to room temperature3N4/ CuO solution, then first Separating-purifying is filtered with 3~5 deionized waters and 1~3 ethyl alcohol afterwards, finally 12h is dried in 60 DEG C of baking ovens, obtains g-C3N4/CuO Powder；
4) g-C for obtaining step 3)3N4/ CuO powder 250 DEG C of heat treatment 2h in Muffle furnace, obtain the g- of high-crystallinity C3N4/ CuO composite material.
Scanning electron microscope (SEM) figure of final product obtained by the present embodiment is shown in Fig. 6, shows g-C in figure3N4/ CuO composite material Pattern is uniform, is in 400~500nm nano particle microballoon.
Embodiment 4
A kind of fabricated in situ g-C3N4The method of/CuO composite material, includes the following steps:
1) 40mL acetonitrile and 10mLN are weighed, dinethylformamide (DMF) is mixed in 250mL beaker, must mix Reaction dissolvent；
2) it weighs 1.5g dicyan diamino and 1.293g copper nitrate is dissolved in mixed reaction solvent obtained by step 1) that (magnetic force stirs Mix 2h), obtain precursor solution；
3) precursor solution for obtaining step 2) is transferred in the reaction kettle of 100mL polytetrafluoroethyllining lining and is heated to 180 DEG C of progress solvent thermal reaction 12h, obtain the g-C of black after reaction kettle naturally cools to room temperature3N4/ CuO solution, then first Separating-purifying is filtered with 3~5 deionized waters and 1~3 ethyl alcohol afterwards, finally 12h is dried in 60 DEG C of baking ovens, obtains g-C3N4/CuO Powder；
4) g-C for obtaining step 3)3N4/ CuO powder 300 DEG C of heat treatment 2h in Muffle furnace, obtain the g- of high-crystallinity C3N4/ CuO composite material.
Scanning electron microscope (SEM) figure of final product obtained by the present embodiment is shown in Fig. 7, shows g-C in figure3N4/ CuO composite material Pattern is uniform, is in 400~500nm nano particle microballoon.
Embodiment 5
A kind of fabricated in situ g-C3N4The method and application of/CuO composite material, include the following steps:
1) 40mL acetonitrile and 10mLN are weighed, dinethylformamide (DMF) is mixed in 250mL beaker, must mix Reaction dissolvent；
2) it weighs 1.5g dicyan diamino and 2.155g copper nitrate is dissolved in mixed reaction solvent obtained by step 1) that (magnetic force stirs Mix 2h), obtain precursor solution；
3) precursor solution for obtaining step 2) is transferred in the reaction kettle of 100mL polytetrafluoroethyllining lining and is heated to 220 DEG C of progress solvent thermal reaction 6h, obtain the g-C of black after reaction kettle naturally cools to room temperature3N4/ CuO solution, then first Separating-purifying is filtered with 3~5 deionized waters and 1~3 ethyl alcohol afterwards, finally 12h is dried in 60 DEG C of baking ovens, obtains g-C3N4/CuO Powder；
4) g-C for obtaining step 3)3N4/ CuO powder 300 DEG C of heat treatment 3h in Muffle furnace, obtain the g- of high-crystallinity C3N4/ CuO composite material.
Scanning electron microscope (SEM) figure of final product obtained by the present embodiment is shown in Fig. 8, shows g-C in figure3N4/ CuO composite material Pattern is uniform, is in 400~500nm nanometer sheet microballoon.
The foregoing is merely the preferred embodiment of the present invention, it is noted that comes for those of ordinary skill in the art It says, without departing from the concept of the premise of the invention, make several modifications and variations, these belong to protection model of the invention It encloses.

Claims (9)

1. a kind of fabricated in situ g-C3N4The method of/CuO composite material, which comprises the steps of:
1) acetonitrile and n,N-Dimethylformamide are stirred evenly, obtains mixed reaction solvent；
2) dicyan diamino and copper nitrate stirring and dissolving in the mixed reaction solvent obtained by step 1), are obtained into precursor solution；
3) gained precursor solution is heated and carries out solvent thermal reaction, then carried out separating-purifying drying, obtain g-C3N4/ CuO powder End；
4) g-C for obtaining step 3)3N4/ CuO powder is placed in Muffle furnace the g-C being heat-treated to get high-crystallinity3N4/ CuO composite material.
2. fabricated in situ g-C according to claim 13N4The method of/CuO composite material, which is characterized in that the acetonitrile and The volume ratio of organic solvent is 1:(0.05~5.0).
3. fabricated in situ g-C according to claim 13N4The method of/CuO composite material, which is characterized in that the dicyan two The molar ratio of ammonia and copper nitrate is 1:(0.1~1.0).
4. fabricated in situ g-C according to claim 13N4The method of/CuO composite material, which is characterized in that institute in step 1) Stating the stirring and dissolving time is 0.5~6h.
5. fabricated in situ g-C according to claim 13N4The method of/CuO composite material, which is characterized in that the solvent heat Reaction temperature is 150~220 DEG C, and the reaction time is 6~48h.
6. fabricated in situ g-C according to claim 13N4The method of/CuO composite material, which is characterized in that the solvent heat Reaction temperature be 180~200 DEG C, the reaction time be 12~for 24 hours.
7. fabricated in situ g-C according to claim 13N4The method of/CuO composite material, which is characterized in that the heat treatment Temperature is 250~350 DEG C, and the time is 1~4h.
8. the g-C of any one of claim 1~7 the method preparation3N4/ CuO composite material, which is characterized in that it is in nano wire Microballoon, nano particle microballoon or nanometer sheet micro-sphere structure, having a size of 400~500nm.
9. g-C described in claim 83N4Application of/CuO the composite material in negative electrode of lithium ion battery.
CN201611219983.3A 2016-12-26 2016-12-26 A kind of method of fabricated in situ graphite phase carbon nitride-oxidation carbon/carbon-copper composite material Expired - Fee Related CN106602023B (en)

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