CN106602023A - Method for in-situ synthesis of graphite phase carbon nitride-copper oxide composite material - Google Patents
Method for in-situ synthesis of graphite phase carbon nitride-copper oxide composite material Download PDFInfo
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- CN106602023A CN106602023A CN201611219983.3A CN201611219983A CN106602023A CN 106602023 A CN106602023 A CN 106602023A CN 201611219983 A CN201611219983 A CN 201611219983A CN 106602023 A CN106602023 A CN 106602023A
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- H01M4/00—Electrodes
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- H—ELECTRICITY
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- H—ELECTRICITY
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- 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a method for in-situ synthesis of a g-C<3>N<4>/Cuo composite material. The method comprises the following steps of 1) uniformly stirring acetonitrile and an organic solvent to obtain a mixed reaction solvent; 2) stirring and dissolving dicyandiamide and copper nitrate into the mixed reaction solvent obtained in the step 1) to obtain a precursor solution; and 3) heating the precursor solution to perform a solvent thermal reaction, and then performing separating, purifying and drying to obtain the g-C<3>N<4>/Cuo composite material. The preparation method is simple, the reaction conditions are mild, and the procedure is simple; and the prepared g-C<3>N<4>/Cuo composite material has lithium storage performance with high circulation stability and high electrode specific capacity, and can be used as a negative electrode material of a lithium ion battery.
Description
Technical field
The invention belongs to the exploitation of new energy materialses and studying technological domain, and in particular to a kind of fabricated in situ graphite-phase nitrogen
Change method and the application of carbon-oxidation carbon/carbon-copper composite material.
Background technology
Lithium ion battery as energy conversion device of new generation, due to its high-energy-density, invertibity and cycle life
The significant advantage such as long is widely studied.In order to meet the requirement of high-energy-density and high power density, exploitation has height
The negative material of high rate performance and high security, to replace traditional Carbon anode, it has also become a urgent task.Carbon anode by
Seriously limit in its relatively low 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 as ion cathode material lithium, its theoretical capacity
It it is more than 2 times of plumbago-carbon negative pole material for 674mA h/g.At present, the cyclical stability of pure phase CuO negative material is not high, leads to
Compound coating is carried out frequently with Graphene, conducting polymer and other materials, the electric conductivity and structural stability for improving CuO is 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, it has good electric conductivity and higher theoretical capacity, therefore g-C3N4/ CuO composites are used for
Lithium-ion negative pole has very big research and using value.
The preparation method of composite can be divided into one-step method and method of fractional steps synthesis.At present, g-C is prepared3N4/ CuO composite woods
The method of material is mainly the method for fractional steps.Method of fractional steps synthetic composite material has second and mutually disperses uneven, and interface cohesion is insecure etc.
Problem.Interface free from admixture pollution of the second of one-step synthesis method composite mutually and between matrix, there is between the two preferable original position
Matching, can significantly improve the bonding state of two-phase interface in material, make material have excellent physical and chemical performance.At present, one
The technical deficiency of footwork synthesis, is difficult nucleation and the growth for regulating and controlling various crystalline phases simultaneously in same system, obtains
Product is typically only physical mixed, cannot get two-phase or multiphase composite, greatly reduces the performance of composite.One step
Method fabricated in situ g-C3N4/ CuO composites have excellent interface fine structure, can be effectively reduced the embedding lithium of battery charging and discharging-
The adverse effect that Volume Changes are brought during de- lithium, the structure of stabilizing actives improves cycle life.
The content of the invention
Present invention aims to the deficiencies in the prior art, there is provided a kind of fabricated in situ g-C3N4/ CuO composites
Method, simple process that the method is related to, reaction condition be gentle, the g-C of preparation3N4/ CuO composites have stable circulation
Property good, the storage lithium performance that electrode specific capacity is high, be adapted to popularization and application.
To achieve these goals, the technical solution used in the present invention is：
A kind of fabricated in situ g-C3N4The method of/CuO composites, comprises the steps：
1) acetonitrile and organic solvent are stirred, obtains mixed reaction solvent；
2) by dicyan diamino and copper nitrate stirring and dissolving in step 1) gained mixed reaction solvent in, obtain precursor solution；
3) heating of gained precursor solution is carried out into solvent thermal reaction, then carries out separating-purifying drying, obtain g-C3N4/CuO
Powder；
4) by step 3) g-C that obtains3N4/ CuO powder is placed in Muffle furnace and is heat-treated (annealing), obtains final product height
The g-C of degree of crystallinity3N4/ CuO composites (graphite phase carbon nitride-oxidation carbon/carbon-copper composite material).
In such scheme, the organic solvent is DMF (DMF).
In such scheme, the volume ratio of the acetonitrile and organic solvent is 1:(0.05～5.0).
In such scheme, the mol ratio of the dicyan diamino and copper nitrate is 1:(0.1～1.0).
Preferably, the copper nitrate and the mass ratio of DMF are 1:(3～15).
In such scheme, step 1) described in the stirring and dissolving time be 0.5～6h.
In such scheme, the solvent thermal reaction temperature is 150～220 DEG C, and the reaction time is 6～48h.
Preferably, the solvent thermal reaction temperature is 180～200 DEG C, and the reaction time is 12～24h.
In such scheme, the heat treatment temperature is 250～350 DEG C, and the time is 1～4h.
The g-C according to obtained in such scheme3N4/ CuO composites, it is in nano wire microballoon, nano particle microballoon or nanometer
Piece micro-sphere structure, the micro-sphere structure being respectively made up of nano wire, nano particle, nanometer sheet, Microsphere Size is 400～500nm；
Ratio or solvent heat temperature, the time for changing reactant, the microscopic appearance of controlled material can be passed through.
G-C described in such scheme3N4Application of/CuO the composites in lithium ion battery negative.
The present invention, with dicyan diamino and copper nitrate as primary raw material, is anti-with acetonitrile and DMF (DMF)
Answer solvent.Acetonitrile promotes dicyan diamino that polycondensation reaction occurs, with the carrying out of polycondensation reaction, the amido in dicyan diamino strand
There is disconnected strong abjection, amido and water reaction generate ammoniacal liquor and OH-, make the aobvious alkalescence of solution；N,N-dimethylformamide (DMF) and nitre
There is complex reaction in sour copper, control crystal grain is grown up, while and g-C3N4The OH that polycondensation deaminizating is produced-Reaction, first generates Cu
(OH)2Precipitation, final reaction generates CuO, and the synergy of the two finally gives the g-C of In-situ reaction3N4/ CuO composites,
The complex crystallization that solvent heat is obtained is relatively low, and by follow-up thermal anneal process the crystallinity of material is improved.
Compared with prior art, beneficial effects of the present invention are：Preparation method according to the present invention is simple, reaction condition temperature
Easy, the g-C of preparation with, operation3N4/ CuO composites have the high storage lithium performance of good cycling stability, electrode specific capacity.
Description of the drawings
Fig. 1 is X-ray diffraction (XRD) figure of the gained final product of the embodiment of the present invention 1.
Fig. 2 is ESEM (SEM) figure of the gained final product of the embodiment of the present invention 1.
Fig. 3 is the cycle performance of lithium ion battery figure of the gained final product of the embodiment of the present invention 1.
Fig. 4 is X-ray diffraction (XRD) figure of the gained final product of the embodiment of the present invention 2.
Fig. 5 is ESEM (SEM) figure of the gained final product of the embodiment of the present invention 2.
Fig. 6 is ESEM (SEM) figure of the gained final product of the embodiment of the present invention 3.
Fig. 7 is ESEM (SEM) figure of the gained final product of the embodiment of the present invention 4.
Fig. 8 is ESEM (SEM) figure of the gained final product of the embodiment of the present invention 5.
Specific embodiment
For a better understanding of the present invention, present disclosure is further elucidated with reference to example, but the present invention is not only
It is limited only to the following examples.
In following examples, the reagent for adopting as no specific instructions is commercially available chemical reagent.
Embodiment 1
A kind of fabricated in situ g-C3N4The method of/CuO composites, comprises the steps：
1) 40mL acetonitriles and 10mL DMFs (DMF) are weighed to mix in 250mL beakers, obtains mixed
Close reaction dissolvent；
2) weigh 1.5g dicyan diamino and 2.155g copper nitrates be dissolved in step 1) gained mixed reaction solvent in (magnetic force is stirred
Mix 2h), obtain precursor solution；
3) by step 2) precursor solution that obtains is transferred in 100mL teflon-lined reactors and is heated to
200 DEG C carry out solvent thermal reaction 24h, and question response kettle naturally cools to the g-C that black is obtained after room temperature3N4/ CuO solution, Ran Houxian
Afterwards with 3～5 deionized waters and 1～3 ethanol suction filtration separating-purifying, most after 60 DEG C of oven for drying 12h, g-C is obtained3N4/CuO
Powder；
4) by step 3) g-C that obtains3N4/ CuO powder is placed in Muffle furnace and is heated to 300 DEG C of heat treatment 2h, obtains highly crystalline
The g-C of degree3N4/ CuO composites.
The XRD spectrum of the present embodiment gained final product is shown in Fig. 1, and g-C is shown in figure3N4It is obvious with the diffraction maximum of CuO, knot
Brilliant degree is high；Fig. 2 is ESEM (SEM) figure of the present embodiment gained final product, and g-C is shown in figure3N4/ CuO composites
Pattern is homogeneous, in 400～500nm nano wire microballoons；Fig. 3 is that the lithium ion battery discharge and recharge of the present embodiment gained final product is followed
Ring performance map, shows that it has the high chemical property of good cycling stability, electrode specific capacity in figure.
Embodiment 2
A kind of fabricated in situ g-C3N4The method of/CuO composites and application, comprise the steps：
1) 33.3mL acetonitriles and 16.7mLN are weighed, dinethylformamide (DMF) is mixed in 250mL beakers, obtained
Mixed reaction solvent；
2) weigh 1.5g dicyan diamino and 2.155g copper nitrates be dissolved in step 1) gained mixed reaction solvent in (magnetic force is stirred
Mix 2h), obtain precursor solution；
3) by step 2) precursor solution that obtains is transferred in 100mL teflon-lined reactors and is heated to
200 DEG C carry out solvent thermal reaction 24h, and question response kettle naturally cools to the g-C that black is obtained after room temperature3N4/ CuO solution, Ran Houxian
Afterwards with 3～5 deionized waters and 1～3 ethanol suction filtration separating-purifying, most after 60 DEG C of oven for drying 12h, g-C is obtained3N4/CuO
Powder；
4) by step 3) g-C that obtains3N4/ CuO powder 300 DEG C of heat treatment 2h in Muffle furnace, obtain the g- of high-crystallinity
C3N4/ CuO composites.
The XRD spectrum of the present embodiment gained final product is shown in Fig. 4, and g-C is shown in figure3N4It is obvious with the diffraction maximum of CuO, knot
Crystalline substance is high；Fig. 5 is ESEM (SEM) figure of the present embodiment gained final product, and g-C is shown in figure3N4/ CuO composite shapes
Looks are homogeneous, in 400～500nm nanometer sheet microballoons.
Embodiment 3
A kind of fabricated in situ g-C3N4The method of/CuO composites and application, comprise the steps：
1) 40mL acetonitriles and 10mLN are weighed, dinethylformamide (DMF) is mixed in 250mL beakers, must mixed
Reaction dissolvent；
2) weigh 1.5g dicyan diamino and 2.155g copper nitrates be dissolved in step 1) gained mixed reaction solvent in (magnetic force is stirred
Mix 2h), obtain precursor solution；
3) by step 2) precursor solution that obtains is transferred in 100mL teflon-lined reactors and is heated to
150 DEG C carry out solvent thermal reaction 24h, and question response kettle naturally cools to the g-C that black is obtained after room temperature3N4/ CuO solution, Ran Houxian
Afterwards with 3～5 deionized waters and 1～3 ethanol suction filtration separating-purifying, most after 60 DEG C of oven for drying 12h, g-C is obtained3N4/CuO
Powder；
4) by step 3) g-C that obtains3N4/ CuO powder 250 DEG C of heat treatment 2h in Muffle furnace, obtain the g- of high-crystallinity
C3N4/ CuO composites.
ESEM (SEM) figure of the present embodiment gained final product is shown in Fig. 6, and g-C is shown in figure3N4/ CuO composites
Pattern is homogeneous, in 400～500nm nano particle microballoons.
Embodiment 4
A kind of fabricated in situ g-C3N4The method of/CuO composites, comprises the steps：
1) 40mL acetonitriles and 10mLN are weighed, dinethylformamide (DMF) is mixed in 250mL beakers, must mixed
Reaction dissolvent；
2) weigh 1.5g dicyan diamino and 1.293g copper nitrates be dissolved in step 1) gained mixed reaction solvent in (magnetic force is stirred
Mix 2h), obtain precursor solution；
3) by step 2) precursor solution that obtains is transferred in 100mL teflon-lined reactors and is heated to
180 DEG C carry out solvent thermal reaction 12h, and question response kettle naturally cools to the g-C that black is obtained after room temperature3N4/ CuO solution, Ran Houxian
Afterwards with 3～5 deionized waters and 1～3 ethanol suction filtration separating-purifying, most after 60 DEG C of oven for drying 12h, g-C is obtained3N4/CuO
Powder；
4) by step 3) g-C that obtains3N4/ CuO powder 300 DEG C of heat treatment 2h in Muffle furnace, obtain the g- of high-crystallinity
C3N4/ CuO composites.
ESEM (SEM) figure of the present embodiment gained final product is shown in Fig. 7, and g-C is shown in figure3N4/ CuO composites
Pattern is homogeneous, in 400～500nm nano particle microballoons.
Embodiment 5
A kind of fabricated in situ g-C3N4The method of/CuO composites and application, comprise the steps：
1) 40mL acetonitriles and 10mLN are weighed, dinethylformamide (DMF) is mixed in 250mL beakers, must mixed
Reaction dissolvent；
2) weigh 1.5g dicyan diamino and 2.155g copper nitrates be dissolved in step 1) gained mixed reaction solvent in (magnetic force is stirred
Mix 2h), obtain precursor solution；
3) by step 2) precursor solution that obtains is transferred in 100mL teflon-lined reactors and is heated to
220 DEG C carry out solvent thermal reaction 6h, and question response kettle naturally cools to the g-C that black is obtained after room temperature3N4/ CuO solution, Ran Houxian
Afterwards with 3～5 deionized waters and 1～3 ethanol suction filtration separating-purifying, most after 60 DEG C of oven for drying 12h, g-C is obtained3N4/CuO
Powder；
4) by step 3) g-C that obtains3N4/ CuO powder 300 DEG C of heat treatment 3h in Muffle furnace, obtain the g- of high-crystallinity
C3N4/ CuO composites.
ESEM (SEM) figure of the present embodiment gained final product is shown in Fig. 8, and g-C is shown in figure3N4/ CuO composites
Pattern is homogeneous, in 400～500nm nanometer sheet microballoons.
The foregoing is only the preferred embodiment of the present invention, it is noted that for one of ordinary skill in the art comes
Say, without departing from the concept of the premise of the invention, make some modifications and variations, these belong to the protection model of the present invention
Enclose.
Claims (10)
1. a kind of fabricated in situ g-C3N4The method of/CuO composites, it is characterised in that comprise the steps：
1) acetonitrile and organic solvent are stirred, obtains mixed reaction solvent；
2) by dicyan diamino and copper nitrate stirring and dissolving in step 1) gained mixed reaction solvent in, obtain precursor solution；
3) heating of gained precursor solution is carried out into solvent thermal reaction, then carries out separating-purifying drying, obtain g-C3N4/ CuO powder
End；
4) by step 3) g-C that obtains3N4/ CuO powder is placed in Muffle furnace and is heat-treated, and obtains final product the g-C of high-crystallinity3N4/
CuO composites.
2. fabricated in situ g-C according to claim 13N4The method of/CuO composites, it is characterised in that described organic molten
Agent is N,N-dimethylformamide.
3. fabricated in situ g-C according to claim 13N4The method of/CuO composites, it is characterised in that the acetonitrile and
The volume ratio of organic solvent is 1:(0.05～5.0).
4. fabricated in situ g-C according to claim 13N4The method of/CuO composites, it is characterised in that the dicyan two
The mol ratio of ammonia and copper nitrate is 1:(0.1～1.0).
5. fabricated in situ g-C according to claim 13N4The method of/CuO composites, it is characterised in that step 1) in institute
The stirring and dissolving time is stated for 0.5～6h.
6. fabricated in situ g-C according to claim 13N4The method of/CuO composites, it is characterised in that the solvent heat
Reaction temperature is 150～220 DEG C, and the reaction time is 6～48h.
7. fabricated in situ g-C according to claim 13N4The method of/CuO composites, it is characterised in that the solvent heat
Reaction temperature is 180～200 DEG C, and the reaction time is 12～24h.
8. fabricated in situ g-C according to claim 13N4The method of/CuO composites, it is characterised in that the heat treatment
Temperature is 250～350 DEG C, and the time is 1～4h.
9. the g-C that prepared by any one of claim 1～8 methods described3N4/ CuO composites, it is characterised in that it is in nano wire
Microballoon, nano particle microballoon or nanometer sheet micro-sphere structure, size is 400～500nm.
10. g-C described in claim 93N4Application of/CuO the composites in lithium ion battery negative.
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| CN109524639A (en) * | 2018-10-16 | 2019-03-26 | 华南师范大学 | Lithium ion battery g-C is prepared using electrostatic spinning3N4The method and its application of/silicon-carbon cathode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107634207A (en) * | 2017-09-19 | 2018-01-26 | 大连海事大学 | A kind of silicon mosaic redox graphene/graphite phase carbon nitride composite and its preparation and application |
| CN108823596A (en) * | 2018-06-11 | 2018-11-16 | 浙江大学 | Gas-diffusion electrode and preparation method thereof and the application in Carbon dioxide electrochemical reduction |
| CN109065873A (en) * | 2018-08-17 | 2018-12-21 | 东莞市凯金新能源科技股份有限公司 | A kind of preparation method and material of the mesoporous graphitic nitralloy carbon negative pole material of loaded nano-copper |
| CN109065873B (en) * | 2018-08-17 | 2021-10-22 | 广东凯金新能源科技股份有限公司 | Preparation method and material of supported nano-copper mesoporous graphite carbon nitride negative electrode material |
| CN109524639A (en) * | 2018-10-16 | 2019-03-26 | 华南师范大学 | Lithium ion battery g-C is prepared using electrostatic spinning3N4The method and its application of/silicon-carbon cathode material |
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| CN110148735A (en) * | 2019-06-03 | 2019-08-20 | 河南师范大学 | A kind of preparation method of self-supporting graphite phase carbon nitride/conducting polymer composite sulfur positive electrode |
| CN110148735B (en) * | 2019-06-03 | 2022-03-22 | 河南师范大学 | Preparation method of self-supporting graphite phase carbon nitride/conductive polymer composite sulfur positive electrode material |
| CN110429246A (en) * | 2019-06-26 | 2019-11-08 | 合肥国轩高科动力能源有限公司 | One type graphite phase carbon nitride coating alpha-Fe2O3Material and preparation method thereof, application |
| CN110429246B (en) * | 2019-06-26 | 2022-06-07 | 合肥国轩高科动力能源有限公司 | alpha-Fe uniformly coated by graphite-like phase carbon nitride2O3Material, and preparation method and application thereof |
| CN113860352A (en) * | 2021-09-25 | 2021-12-31 | 河北工程大学 | Preparation method of nano copper oxide-graphite phase carbon nitride composite material and drying device for preparation |
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