CN108417803A - A kind of N doping hollow carbon sphere composite material and preparation method and application - Google Patents
A kind of N doping hollow carbon sphere composite material and preparation method and application Download PDFInfo
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Abstract
The invention belongs to field of lithium ion battery material, a kind of N doping hollow carbon sphere composite material and preparation method and application are disclosed.By manganese acetate and ammonium bicarbonate solubility in ethylene glycol, solvent thermal reaction is carried out at a temperature of 180~220 DEG C, obtain manganese carbonate, it is reacted again with Dopamine hydrochloride, manganese carbonate/poly-dopamine composite material is obtained, then calcination processing under an inert atmosphere, obtains nitrogen-doped carbon coated manganese oxide composite material, finally handled with acid solution, wash, dry after obtain the N doping hollow carbon sphere composite material.The preparation method of the present invention is simple, of low cost, environmental-friendly.Prepared N doping hollow carbon sphere composite structure is stablized, and conducts electricity very well, and has excellent stable circulation performance as lithium ion battery negative material.
Description
Technical field
The invention belongs to field of lithium ion battery material, and in particular to a kind of N doping hollow carbon sphere composite material and its system
Preparation Method and application.
Background technology
Three big themes of 21st century scientific technological advance are the energy, environment and information, wherein the scarcity of the energy and
Serious problem of environmental pollution has become two hang-ups urgently to be resolved hurrily.The energy and environment are that the mankind depend on for existence and development
Important foundation, it is closely bound up with the sustainable development of human society.Energy exploitation and application pattern based on primary energy and life
A series of energy and environment such as the contradiction between state environment is increasingly sharpened, and fossil energy is petered out, environmental pollution is on the rise
Problem seriously threatens the survival and development of the mankind.Currently, people's demand growing to the energy depends on oil, day
The right traditional energies such as gas and coal.With the consumption of the non-renewable resources such as fossil fuel, energy shortage problem has become
The problem that 21 century people must solve.Therefore, countries in the world government actively develops efficient, safe, green New Energy one after another
Source and new energy materials.In order to cope with above two hang-up, people are dedicated to developing the novel green cleaning such as solar energy, wind energy
The energy, to gradually replace fossil class A fuel A that is non-renewable and causing environmental pollution.However, due to wind energy and solar energy
Source disperses and unstable, and efficiently, therefore green, practical energy storage device times paid high attention to by countries in the world.
Currently, the secondary cell used mainly has：Four kinds of Ni-MH battery, nickel-cadmium cell, lead-acid battery and lithium ion battery.
Since lead-acid battery and nickel-cadmium cell are related to the use of toxic metals lead and cadmium in use, in environmental consciousness day
Their use today that benefit improves is subject to certain restrictions, and Ni-MH battery is since its performance is far from meeting the needs of people
Its research is set increasingly to decay.Lithium ion battery have operating voltage is high, energy density is high, have extended cycle life, memory-less effect with
And the advantages that environmentally protective, it is current classic novel environment friendly secondary cell.
Currently, the commercialization of the negative material of lithium ion battery is based on traditional graphite carbon-based material, but its theoretical ratio
The relatively low only 372mAhg of capacity-1, it cannot meet requirement of the electrical equipment to energy density and power density, therefore there is an urgent need to
High performance ion cathode material lithium.Therefore, it is extremely urgent to develop lithium ion battery negative material of new generation.Hollow carbon material tool
There is unique structure, and thermal stability and chemical stability are preferable, manufacturing cost is low, is answered in terms of lithium ion battery electrode material
With extensive.In addition, in order to make carbon material have higher lithium ion storge quality, nitrogen-doping is considered proper
Method.Until up to now, there are no the relevant reports of N doping hollow carbon sphere.
Invention content
It is relatively low for traditional itself theoretical capacity of carbons negative material at present, it is more difficult to the feelings to satisfy the needs of the people
Condition, the primary purpose of the present invention is that providing a kind of preparation method of N doping hollow carbon sphere composite material.The present invention utilizes acid
Nitrogen-doped carbon coated manganese oxide composite material is carried out acidification by facture, obtains N doping hollow carbon sphere (Hollow
Carbon spheres) composite material.This method can improve the structural stability of material, to improve the electrochemistry of negative material
Performance.
Another object of the present invention is to provide a kind of N doping hollow carbon sphere being prepared by the above method is compound
Material.
It is still another object of the present invention to provide above-mentioned N doping hollow carbon sphere composite materials in negative electrode of lithium ion battery material
Application in material.
The object of the invention is achieved through the following technical solutions：
A kind of preparation method of N doping hollow carbon sphere (Hollow carbon spheres) composite material, including it is as follows
Preparation process：
(1) manganese acetate and ammonium bicarbonate solubility are subjected to solvent thermal reaction in ethylene glycol at a temperature of 180~220 DEG C,
Product is washed, dry, obtains manganese carbonate micron ball；
(2) manganese carbonate micron ball is dissolved in Dopamine hydrochloride in Tris buffer solutions and is reacted, solid product is washed,
It is dry, obtain manganese carbonate/poly-dopamine composite material；
(3) it by the calcination processing under an inert atmosphere of manganese carbonate/poly-dopamine composite material obtained by step (2), obtains nitrogen and mixes
Miscellaneous carbon coating manganese oxide composite material；
(4) nitrogen-doped carbon coated manganese oxide obtained by step (3) is handled with acid solution, wash, dry after obtain institute
State N doping hollow carbon sphere composite material.
Preferably, the molar ratio of manganese acetate and ammonium hydrogen carbonate described in step (1) is 1:(8~12).
Preferably, the mass ratio of manganese carbonate micron ball and Dopamine hydrochloride described in step (2) is 1:(1~3).
Preferably, Tris buffer solutions described in step (2) refer to the Tris buffer solutions of pH=8.5.
Preferably, inert atmosphere described in step (3) refers to nitrogen atmosphere.
Preferably, calcination processing described in step (3) refers to first calcining 5~8h at 700~800 DEG C, then it is cooled to
400~500 DEG C are persistently calcined 2~3h again.
Preferably, the acid solution described in step (4) is at least one of sulfuric acid, hydrochloric acid and oxalic acid solution.
Preferably, a concentration of 0.1~1mol/L of acid solution described in step (4).
Preferably, the time of the processing of acid solution described in step (4) is 12~48h.
A kind of N doping hollow carbon sphere composite material, is prepared by the above method.The N doping hollow carbon sphere is compound
The grain size of material is 400~600nm.
Application of the above-mentioned N doping hollow carbon sphere composite material in lithium ion battery negative material.
The present invention preparation method and obtained product has the following advantages that and advantageous effect：
(1) preferable electrification is made it have to further improve the electric conductivity of material due to the doping of nitrogen
Learn activity；
(2) since carbon ball is existed in the form of hollow, it can suitably alleviate the volume expansion in charge and discharge process, make electricity
Pond has preferable cyclical stability；
(3) polymerization of dopamine of the present invention is very simple, it is only necessary to be carried out under room temperature and weak basic condition, cost
It is relatively low, environmental-friendly, the development of scale lithium ion battery negative material can be promoted, be expected to large-scale industrialization application.
Description of the drawings
Fig. 1 is the XRD diagram of gained N doping hollow carbon sphere composite material in the embodiment of the present invention 1.
Fig. 2 is the N- adsorption/desorption figures of gained N doping hollow carbon sphere composite material in the embodiment of the present invention 1.
Fig. 3 is the XPS figures of gained N doping hollow carbon sphere composite material in the embodiment of the present invention 1.
Fig. 4 is the SEM figures of gained N doping hollow carbon sphere composite material in the embodiment of the present invention 1.
Fig. 5 is the TEM figures of gained N doping hollow carbon sphere composite material in the embodiment of the present invention 1.
Fig. 6 is gained N doping hollow carbon sphere composite material in the embodiment of the present invention 1 as lithium ion battery negative material
Constant current charge-discharge performance map.
Fig. 7 is gained N doping hollow carbon sphere composite material in the embodiment of the present invention 1 as lithium ion battery negative material
Recycle the constant current charge-discharge performance map after 100 weeks.
Fig. 8 is gained N doping hollow carbon sphere composite material in the embodiment of the present invention 1 as lithium ion battery negative material
Constant current charge-discharge performance map under high current.
Specific implementation mode
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) in the ammonium bicarbonate solubility of the manganese acetate of 1mmol and 10mmol to the ethylene glycol solution of 30mL, at 180 DEG C
Hydro-thermal reaction 12h is carried out, after being cooled to room temperature, then centrifuge washing, it is dry, obtain manganese carbonate micron ball.
(2) the manganese carbonate micron ball of 100mg and 100mg Dopamine hydrochlorides are dissolved in the Tris buffer solutions of pH ≈ 8.5,
Room temperature is reacted, then reaction product is separated by solid-liquid separation, and washs solid, dry, obtains manganese carbonate/poly-dopamine compound.
(3) under nitrogen protection, manganese carbonate/poly-dopamine compound is calcined into 5h at 700 DEG C, then cools to 500 DEG C, then
Sustained response 2h obtains nitrogen-doped carbon coated manganese oxide particle.
(4) the sulfuric acid treatment nitrogen-doped carbon coated manganese oxide particle for using 0.5mol/L for 24 hours, with absolute ethyl alcohol centrifugation, is dried,
Obtain N doping hollow carbon sphere composite material.
Fig. 1 is the XRD diagram of N doping hollow carbon sphere composite material obtained by the present embodiment.X-ray powder diffraction (XRD) is analyzed
Show that the product of gained is pure carbon, does not find dephasign, illustrate that purity is higher.Fig. 2 is the hollow carbon of N doping obtained by the present embodiment
The N- adsorption/desorption figures of ball composite material.Specific surface area analysis shows that the specific surface area of products therefrom is 201m2g-1, have larger
Specific surface area.Fig. 3 is the XPS figures of N doping hollow carbon sphere composite material obtained by the present embodiment.It can from XPS analysis
It arrives, there is the presence of carbon and nitrogen.Fig. 4 and Fig. 5 is respectively N doping hollow carbon sphere composite material obtained by the present embodiment
SEM schemes and TEM figures.It is hollow from scanning electron microscope (SEM) and transmission electron microscope (TEM) it can be seen from the figure that resulting product
Carbon ball, grain size be 400~600nm.
N doping hollow carbon sphere composite material obtained by the present embodiment is surveyed as the application performance of lithium ion battery negative material
Examination：
Using obtained N doping hollow carbon sphere as active material, acetylene black is conductive agent, and Kynoar is binder,
And according to active material:Conductive agent:Binder=7:2:In the cillin bottle of 1 mass ratio merging 5mL, then it is added dropwise 0.5mL's
N-methyl pyrrolidones stirs pulp after 4h, and slurry is uniformly applied on copper foil, and it is dry to be then put into 80 DEG C of thermostatic drying chamber
Dry 12h, it is working electrode to be gone out as the sequin of 12mm using sheet-punching machine after drying to constant weight, anhydrous in guarantee
Sequin is put into the glove box full of argon gas, the lithium piece of purchase is used as the Celgard used electrode and reference electrode
2400 type diaphragms, electrolyte are 1mol L-1LiPF6With ethylene carbonate (EC), dimethyl carbonate (DMC) (EC:DMC=1:
2, ν/ν) mixed liquor, the button cell of model CR2025 is finally assembled into glove box, the glove box in whole process must
Oxygen and water vapour content must be kept to be respectively less than 1ppm.At a temperature of 25 DEG C, to carry out constant current charge and discharge under the current density of 100mA/g
Electrical testing, Fig. 6 are that N doping hollow carbon sphere composite material obtained by the present embodiment is filled as the constant current of lithium ion battery negative material
Discharge performance figure.Discharge capacity is 975.8mAh/g for the first time for it, and initial charge capacity reaches 531mAh/g.Fig. 7 is the present embodiment
Gained N doping hollow carbon sphere composite material as lithium ion battery negative material recycle 100 weeks after constant current charge-discharge performance
Figure.At a temperature of 25 DEG C, when carrying out constant current charge-discharge test under the current density of 100mA/g, cycle is after 100 weeks, reversible appearance
Amount is 563.2mAh/g.Fig. 8 is N doping hollow carbon sphere composite material obtained by the present embodiment as lithium ion battery negative material
Constant current charge-discharge performance map at a temperature of 25 DEG C and under 1000mA/g high currents.Pass through under the high current density of 1000mA/g
800 charge and discharge, the still reversible capacity with about 390mAh/g, have preferable cyclical stability.
Embodiment 2
(1) in the ammonium bicarbonate solubility of the manganese acetate of 1mmol and 12mmol to the ethylene glycol solution of 30mL, at 200 DEG C
Carry out hydro-thermal reaction for 24 hours, after being cooled to room temperature, then centrifuge washing, it is dry, obtain manganese carbonate micron ball.
(2) the manganese carbonate micron ball of 100mg and 300mg Dopamine hydrochlorides are dissolved in the Tris buffer solutions of pH ≈ 8.5,
Room temperature is reacted, then reaction product is separated by solid-liquid separation, and washs solid, dry, obtains manganese carbonate/poly-dopamine compound.
(3) under nitrogen protection, manganese carbonate/poly-dopamine compound is calcined into 8h at 800 DEG C, then cools to 400 DEG C, then
Sustained response 3h obtains nitrogen-doped carbon coated manganese oxide particle.
(4) the HCl treatment nitrogen-doped carbon coated manganese oxide particle for using 0.1mol/L for 24 hours, with absolute ethyl alcohol centrifugation, is dried,
Obtain N doping hollow carbon sphere composite material.
Button is assembled into using N doping hollow carbon sphere manufactured in the present embodiment (Hollow carbon spheres) and lithium piece
Formula half-cell.At a temperature of 25 DEG C, when carrying out constant current charge-discharge test under the current density of 100mA/g, discharge capacity for the first time
For 865mAh/g, initial charge capacity reaches 449mAh/g.At a temperature of 25 DEG C, constant current is carried out under the current density of 100mA/g
When charge-discharge test, cycle is after 100 weeks, reversible capacity 500mAh/g.It is close in the high current of 1000mA/g at a temperature of 25 DEG C
Under degree, still there is the reversible capacity of about 300mAh/g, there is preferable chemical property.
Embodiment 3
(1) in the ammonium bicarbonate solubility of the manganese acetate of 1mmol and 8mmol to the ethylene glycol solution of 30mL, at 220 DEG C into
Row hydro-thermal reaction 12h, after being cooled to room temperature, then centrifuge washing, it is dry, obtain manganese carbonate micron ball.
(2) the manganese carbonate micron ball of 100mg and 200mg Dopamine hydrochlorides are dissolved in the Tris buffer solutions of pH ≈ 8.5,
Room temperature is reacted, then reaction product is separated by solid-liquid separation, and washs solid, dry, obtains manganese carbonate/poly-dopamine compound.
(3) under nitrogen protection, manganese carbonate/poly-dopamine compound is calcined into 6h at 700 DEG C, then cools to 500 DEG C, then
Sustained response 3h obtains nitrogen-doped carbon coated manganese oxide particle.
(4) the oxalic acid treatment nitrogen-doped carbon coated manganese oxide particle 48h for using 1mol/L is obtained with absolute ethyl alcohol centrifugation, drying
To N doping hollow carbon sphere composite material.
Button is assembled into using N doping hollow carbon sphere manufactured in the present embodiment (Hollow carbon spheres) and lithium piece
Formula half-cell.At a temperature of 25 DEG C, when carrying out constant current charge-discharge test under the current density of 100mA/g, discharge capacity for the first time
For 786mAh/g, initial charge capacity reaches 393mAh/g.At a temperature of 25 DEG C, constant current is carried out under the current density of 100mA/g
When charge-discharge test, cycle is after 100 weeks, reversible capacity 510mAh/g.It is close in the high current of 1000mA/g at a temperature of 25 DEG C
Under degree, still there is the reversible capacity of about 310mAh/g, there is preferable chemical property.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of N doping hollow carbon sphere composite material, it is characterised in that including following preparation process：
(1) manganese acetate and ammonium bicarbonate solubility are subjected to solvent thermal reaction, product in ethylene glycol at a temperature of 180~220 DEG C
It is washed, dry, obtain manganese carbonate micron ball；
(2) manganese carbonate micron ball is dissolved in Dopamine hydrochloride in Tris buffer solutions and is reacted, solid product is washed, dry
It is dry, obtain manganese carbonate/poly-dopamine composite material；
(3) by the calcination processing under an inert atmosphere of manganese carbonate/poly-dopamine composite material obtained by step (2), nitrogen-doped carbon is obtained
Coated manganese oxide composite material；
(4) nitrogen-doped carbon coated manganese oxide obtained by step (3) is handled with acid solution, wash, dry after obtain the nitrogen
Doped hollow carbon ball composite material.
2. a kind of preparation method of N doping hollow carbon sphere composite material according to claim 1, it is characterised in that：Step
(1) molar ratio of manganese acetate described in and ammonium hydrogen carbonate is 1:(8~12).
3. a kind of preparation method of N doping hollow carbon sphere composite material according to claim 1, it is characterised in that：Step
(2) mass ratio of manganese carbonate micron ball described in and Dopamine hydrochloride is 1:(1~3).
4. a kind of preparation method of N doping hollow carbon sphere composite material according to claim 1, it is characterised in that：Step
(2) Tris buffer solutions described in refers to the Tris buffer solutions of pH=8.5.
5. a kind of preparation method of N doping hollow carbon sphere composite material according to claim 1, it is characterised in that：Step
(3) inert atmosphere described in refers to nitrogen atmosphere；The calcination processing refers to that 5~8h is first calcined at 700~800 DEG C, is then dropped
Temperature to 400~500 DEG C again persistently calcine 2~3h.
6. a kind of preparation method of N doping hollow carbon sphere composite material according to claim 1, it is characterised in that：Step
(4) acid solution described in is at least one of sulfuric acid, hydrochloric acid and oxalic acid solution.
7. a kind of preparation method of N doping hollow carbon sphere composite material according to claim 1, it is characterised in that：Step
(4) a concentration of 0.1~1mol/L of acid solution described in.
8. a kind of preparation method of N doping hollow carbon sphere composite material according to claim 1, it is characterised in that：Step
(4) time of the processing of acid solution described in is 12~48h.
9. a kind of N doping hollow carbon sphere composite material, it is characterised in that：Pass through claim 1~8 any one of them method
It is prepared.
10. application of the N doping hollow carbon sphere composite material in lithium ion battery negative material described in claim 9.
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| CN109569687A (en) * | 2018-11-29 | 2019-04-05 | 武汉工程大学 | A kind of stannic oxide with core-shell structure/N doping graphite/cadmium sulfide composite material and preparation method thereof |
| CN109626355A (en) * | 2019-01-14 | 2019-04-16 | 燕山大学 | The production method and its application of situ Nitrogen Doping hollow carbon sphere and preparation method thereof and electrode material |
| CN111063549A (en) * | 2019-12-23 | 2020-04-24 | 南京农业大学 | Two-dimensional MOFs nanosheet-derived full-electrode material for hybrid capacitor |
| CN111211305A (en) * | 2020-01-14 | 2020-05-29 | 南昌大学 | PDA (personal digital Assistant) metal oxide coated high-nickel ternary layered positive electrode material and preparation method thereof |
| CN113332976A (en) * | 2021-05-18 | 2021-09-03 | 贵州大学 | CeCO3OH nanosphere wrapped MnCO3Preparation method and application of microsphere composite material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109569687A (en) * | 2018-11-29 | 2019-04-05 | 武汉工程大学 | A kind of stannic oxide with core-shell structure/N doping graphite/cadmium sulfide composite material and preparation method thereof |
| CN109626355A (en) * | 2019-01-14 | 2019-04-16 | 燕山大学 | The production method and its application of situ Nitrogen Doping hollow carbon sphere and preparation method thereof and electrode material |
| CN111063549A (en) * | 2019-12-23 | 2020-04-24 | 南京农业大学 | Two-dimensional MOFs nanosheet-derived full-electrode material for hybrid capacitor |
| CN111063549B (en) * | 2019-12-23 | 2021-05-18 | 南京农业大学 | Two-dimensional MOFs nanosheet-derived full-electrode material for hybrid capacitor |
| CN111211305A (en) * | 2020-01-14 | 2020-05-29 | 南昌大学 | PDA (personal digital Assistant) metal oxide coated high-nickel ternary layered positive electrode material and preparation method thereof |
| CN111211305B (en) * | 2020-01-14 | 2022-06-10 | 南昌大学 | PDA (personal digital Assistant) metal oxide coated high-nickel ternary layered positive electrode material and preparation method thereof |
| CN113332976A (en) * | 2021-05-18 | 2021-09-03 | 贵州大学 | CeCO3OH nanosphere wrapped MnCO3Preparation method and application of microsphere composite material |
| CN113332976B (en) * | 2021-05-18 | 2022-06-07 | 贵州大学 | CeCO3OH nanosphere wrapped MnCO3Preparation method and application of microsphere composite material |
| CN114159584A (en) * | 2022-02-11 | 2022-03-11 | 中国人民解放军军事科学院军事医学研究院 | Preparation method of manganese-doped hollow carbon spheres with light response performance and application of manganese-doped hollow carbon spheres in antibacterial field |
| CN114159584B (en) * | 2022-02-11 | 2022-04-26 | 中国人民解放军军事科学院军事医学研究院 | Preparation method of manganese-doped hollow carbon spheres with light response performance and application of manganese-doped hollow carbon spheres in antibacterial field |
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