CN109888212A - The preparation method of nitrogen boron codope porous carbon composite - Google Patents
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Abstract
The invention discloses a kind of preparation methods of nitrogen boron codope porous carbon composite, and by the way that para hydroxybenzene boric acid to be dissolved in deionized water, magnetic agitation is uniformly mixed, and obtain para hydroxybenzene boric acid solution；Cyanamide and para hydroxybenzene boric acid solution solution are added dropwise in deionized water simultaneously under magnetic stirring, magnetic agitation is uniformly mixed, and obtains mixed solution；It by mixed solution, is rapidly frozen with liquid nitrogen, is put into drying in freeze drier, obtains white powder, powder is calcined in atmosphere of inert gases, obtain nitrogen boron codope carbon material.The present invention has many advantages, such as that product electrochemical performance, preparation method are simple, at low cost.
Description
Technical field
The present invention relates to the preparation methods of nitrogen boron codope porous carbon composite, belong to carbon material and lithium ion secondary electricity
Pool technology field.
Background technique
Non-renewable fossil energy is largely lost and environmental problem has become hot topic instantly, such as two
It has been that the mankind have beaten alarm bell that the discharge of carbonoxide, which causes greenhouse effects,.It is constantly progressive with economical, industry, the size of population
Increasing, life requirement increasingly increases, and people have closed on that supply falls short of demand to asking for for the energy, and reserves are increasingly poor.This compels
Us are made to find the safe and environmentally friendly new energy of one kind to substitute fossil energy.Green energy resource, such as solar energy, water
Power, heating power and wind energy replace traditional energy at last.In these renewable energy, solar energy and wind energy have certain intermittence.
The appearance of lithium ion battery solves the problems, such as concern that is most important, therefore having focused many scientists, comes in recent years
The development advanced by leaps and bounds, lithium ion battery is due to high energy force density, high power density, long circulation life and not dirty
It contaminates the advantages such as environment and becomes high energy green energy-storing material of new generation.Currently, lithium ion battery have been widely used for it is all kinds of
The energy storage devices such as portable electronic product, wearable electronic product and electric car field.It is currently close to high-energy in order to meet
The eager demand of degree, high power density and stable long circulation life electrode material, research have high theoretical specific capacity and low electricity
The electrode material of flattening bench (cathode) is extremely urgent.
For negative electrode material, negative electrode material graphite (the theoretical capacity 372mA h g of Current commercialization use-1), but its
High rate performance and cycle performance are poor, are not able to satisfy the demand of next-generation high-performance lithium ion battery (LIBs) increasingly.To meet
These demands are badly in need of the negative electrode material that exploitation possesses the advantages that managing big capacity, good rate capability, having extended cycle life.
Summary of the invention
The purpose of the present invention is to propose to a kind of preparation methods of nitrogen boron codope porous carbon composite, total by nitrogen boron
Doping improves porous carbon materials cycle performance.
The present invention is achieved through the following technical solutions:
A kind of preparation method of nitrogen boron codope porous carbon composite, comprising:
Appropriate para hydroxybenzene boric acid is dissolved in deionized water with 1:10 mass ratio, stirring 1h is uniformly mixed it, obtains
Para hydroxybenzene boric acid solution；
The appropriate deionization persistently stirred is added according to volume ratio 1:(0.2-5) for cyanamide and para hydroxybenzene boric acid solution
In water, stirring 1-5h is uniformly mixed it, obtains mixed solution；
It is rapidly frozen mixed solution to form frozen material with liquid nitrogen, and frozen material is put into freeze drier dry (36
~60) h obtains white powder；And
Inert gas is passed through in heating furnace and forms inert atmosphere, and white powder is put into the heating furnace, makes institute
It states heating furnace to carry out temperature programming and white powder is calcined in the heating furnace, it is compound to obtain nitrogen boron codope porous carbon
Material.
In above-mentioned technical proposal, the para hydroxybenzene boric acid concentration is at least 97%.
In above-mentioned technical proposal, the cyanamide concentration is at least 93%.
In above-mentioned technical proposal, the total volume and deionized water volume of the cyanamide and the para hydroxybenzene boric acid solution
Than for 1:(0.5~2).
In above-mentioned technical proposal, the inert gas is nitrogen or argon gas.
In above-mentioned technical proposal, the heating furnace programmed rate is 2-5 DEG C/min, and calcination temperature is 400~800
DEG C, and 0.5~4h of calcination time.
The present invention has the following advantages and beneficial effects: the nitrogen boron being prepared using para hydroxybenzene boric acid and cyanamide is total
Doped porous carbon material, duct is abundant, has excellent chemical property；And preparation method is simple, it is low in cost.
Detailed description of the invention
Fig. 1 is the nitrogen De contamination curve graph of nitrogen boron codope porous carbon composite in embodiment 1.
Fig. 2 is the pore size distribution curve figure of nitrogen boron codope porous carbon composite in embodiment 1.
Fig. 3 is the cycle performance figure of nitrogen boron codope porous carbon composite in embodiment 1.
Specific embodiment
In order to better illustrate the present invention, with reference to the attached drawing in the embodiment of the present invention, in the embodiment of the present invention
Technical solution is clearly and completely described.
The present invention prepares porous carbon composite using nitrogen, boron codope, to improve as the porous of capacitance material
The cycle performance of carbon composite.
Its preparation process includes:
The para hydroxybenzene boric acid that appropriate concentration is at least 97% is dissolved in deionized water with 1:10 mass ratio, stirring 1h makes
It is uniformly mixed, and obtains para hydroxybenzene boric acid solution.
It is 1:(0.2-5 according to the volume ratio of cyanamide and para hydroxybenzene boric acid solution) measure the ammonia that concentration is at least 93%
Base cyanogen, and the cyanamide of measurement and para hydroxybenzene boric acid solution are added together in the deionized water persistently stirred, cyanamide and
The total volume and deionized water volume ratio of para hydroxybenzene boric acid solution are 1:(0.5~2).1~h of stirring is uniformly mixed three,
Obtain mixed solution.
It is rapidly frozen mixed solution to form frozen material with liquid nitrogen, and frozen material is put into freeze drier dry (36
~60) h obtains white powder；And
Nitrogen or argon gas are passed through in heating furnace and form inert atmosphere, and white powder is put into the heating furnace, is made
The heating furnace carries out temperature programming and white powder is made to calcine (0.5~4) h, calcination temperature 400 in the heating furnace
~800 DEG C, obtain nitrogen boron codope porous carbon composite.At this point, heating furnace programmed rate is 2-5 DEG C/min.
Embodiment 1 to 12 each provides the ratio, cold for changing cyanamide and para hydroxybenzene boric acid solution and deionized water
The conditions such as lyophilizer drying time, calcination temperature, calcination atmosphere and calcination time prepare nitrogen boron codope porous carbon materials
(CxNyB)。
Embodiment 1:
(1) 0.4g para hydroxybenzene boric acid is dissolved in 4mL deionized water, magnetic agitation 1h, is uniformly mixed, is obtained para hydroxybenzene
Boric acid solution；
(2) under magnetic stirring, while by 8mL cyanamide and 4mL para hydroxybenzene boric acid solution it is added dropwise to 12mL deionization
In water, magnetic agitation 1h is uniformly mixed, obtains mixed solution；
(3) it by mixed solution obtained above, is rapidly frozen with liquid nitrogen, is put into freeze drier dry 48h, obtains white
Color powder；
(4) by above-mentioned white powder, in argon atmosphere, it is calcined to 3h at 500 DEG C, heating rate is 4 DEG C/min,
Obtain nitrogen boron codope porous carbon materials.
Embodiment 2:
(1) 0.4g para hydroxybenzene boric acid is dissolved in 4mL deionized water, magnetic agitation 1h, is uniformly mixed, is obtained para hydroxybenzene
Boric acid solution；
(2) under magnetic stirring, while by 8mL cyanamide and 4mL para hydroxybenzene boric acid solution it is added dropwise to 6mL deionized water
In, magnetic agitation 1h is uniformly mixed, obtains mixed solution；
(3) it by mixed solution obtained above, is rapidly frozen with liquid nitrogen, is put into freeze drier dry 48h, obtains white
Color powder；
(4) by above-mentioned white powder, in argon atmosphere, it is calcined to 3h at 500 DEG C, heating rate is 4 DEG C/min,
Obtain nitrogen boron codope porous carbon materials.
Embodiment 3:
(1) 0.4g para hydroxybenzene boric acid is dissolved in 4mL deionized water, magnetic agitation 1h, is uniformly mixed, is obtained para hydroxybenzene
Boric acid solution；
(2) under magnetic stirring, while by 8mL cyanamide and 4mL para hydroxybenzene boric acid solution it is added dropwise to 18mL deionization
In water, magnetic agitation 2h is uniformly mixed, obtains mixed solution；
(3) it by mixed solution obtained above, is rapidly frozen with liquid nitrogen, is put into freeze drier dry 48h, obtains white
Color powder；
(4) by above-mentioned white powder, in argon atmosphere, it is calcined to 3h at 500 DEG C, heating rate is 4 DEG C/min,
Obtain nitrogen boron codope porous carbon materials.
Embodiment 4:
(1) 0.6g para hydroxybenzene boric acid is dissolved in 6mL deionized water, magnetic agitation 1h, is uniformly mixed, is obtained para hydroxybenzene
Boric acid solution；
(2) under magnetic stirring, while by 6mL cyanamide and 6mL para hydroxybenzene boric acid solution it is added dropwise to 12mL deionization
In water, magnetic agitation 1h is uniformly mixed, obtains mixed solution；
(3) it by mixed solution obtained above, is rapidly frozen with liquid nitrogen, is put into freeze drier dry 36h, obtains white
Color powder；
(4) by above-mentioned white powder, in argon atmosphere, it is calcined to 3h at 500 DEG C, heating rate is 4 DEG C/min,
Obtain nitrogen boron codope porous carbon materials.
Embodiment 5:
(1) 1g para hydroxybenzene boric acid is dissolved in 10mL deionized water, magnetic agitation 1h, is uniformly mixed, is obtained para hydroxybenzene
Boric acid solution；
(2) under magnetic stirring, while by 2mL cyanamide and 10mL para hydroxybenzene boric acid solution it is added dropwise to 24mL deionization
In water, magnetic agitation 3h is uniformly mixed, obtains mixed solution；
(3) it by mixed solution obtained above, is rapidly frozen with liquid nitrogen, is put into freeze drier dry 60h, obtains white
Color powder；
(4) by above-mentioned white powder, in argon atmosphere, it is calcined to 3h at 500 DEG C, heating rate is 4 DEG C/min,
Obtain nitrogen boron codope porous carbon materials.
Embodiment 6:
(1) 0.8g para hydroxybenzene boric acid is dissolved in 8mL deionized water, magnetic agitation 1h, is uniformly mixed, is obtained para hydroxybenzene
Boric acid solution；
(2) under magnetic stirring, while by 4mL cyanamide and 8mL para hydroxybenzene boric acid solution it is added dropwise to 12mL deionization
In water, magnetic agitation 1h is uniformly mixed, obtains mixed solution；
(3) it by mixed solution obtained above, is rapidly frozen with liquid nitrogen, is put into freeze drier dry 48h, obtains white
Color powder；
(4) by above-mentioned white powder, in nitrogen atmosphere encloses, it is calcined to 3h at 400 DEG C, heating rate is 4 DEG C/
Min obtains nitrogen boron codope porous carbon materials.
Embodiment 7:
(1) 0.3g para hydroxybenzene boric acid is dissolved in 3mL deionized water, magnetic agitation 1h, is uniformly mixed, is obtained para hydroxybenzene
Boric acid solution；
(2) under magnetic stirring, while by 10mL cyanamide and 2mL para hydroxybenzene boric acid solution it is added dropwise to 12mL deionization
In water, magnetic agitation 1h is uniformly mixed, obtains mixed solution；
(3) it by mixed solution obtained above, is rapidly frozen with liquid nitrogen, is put into freeze drier dry 48h, obtains white
Color powder；
(4) by above-mentioned white powder, in argon atmosphere, it is calcined to 3h at 800 DEG C, heating rate is 4 DEG C/min,
Obtain nitrogen boron codope porous carbon materials.
Embodiment 8:
(1) 0.4g para hydroxybenzene boric acid is dissolved in 4mL deionized water, magnetic agitation 1h, is uniformly mixed, is obtained para hydroxybenzene
Boric acid solution；
(2) under magnetic stirring, while by 8mL cyanamide and 4mL para hydroxybenzene boric acid solution it is added dropwise to 12mL deionization
In water, magnetic agitation 5h is uniformly mixed, obtains mixed solution；
(3) it by mixed solution obtained above, is rapidly frozen with liquid nitrogen, is put into freeze drier dry 48h, obtains white
Color powder；
(4) by above-mentioned white powder, in argon atmosphere, it is calcined to 0.5h at 500 DEG C, heating rate is 4 DEG C/
Min obtains nitrogen boron codope porous carbon materials.
Embodiment 9:
(1) 0.4g para hydroxybenzene boric acid is dissolved in 4mL deionized water, magnetic agitation 1h, is uniformly mixed, is obtained para hydroxybenzene
Boric acid solution；
(2) under magnetic stirring, while by 8mL cyanamide and 4mL para hydroxybenzene boric acid solution it is added dropwise to 12mL deionization
In water, magnetic agitation 1h is uniformly mixed, obtains mixed solution；
(3) it by mixed solution obtained above, is rapidly frozen with liquid nitrogen, is put into freeze drier dry 48h, obtains white
Color powder；
(4) by above-mentioned white powder, in argon atmosphere, it is calcined to 4h at 500 DEG C, heating rate is 4 DEG C/min,
Obtain nitrogen boron codope porous carbon materials.
Embodiment 10:
(1) 0.4g para hydroxybenzene boric acid is dissolved in 4mL deionized water, magnetic agitation 1h, is uniformly mixed, is obtained para hydroxybenzene
Boric acid solution；
(2) under magnetic stirring, while by 8mL cyanamide and 4mL para hydroxybenzene boric acid solution it is added dropwise to 12mL deionization
In water, magnetic agitation 1h is uniformly mixed, obtains mixed solution；
(3) it by mixed solution obtained above, is rapidly frozen with liquid nitrogen, is put into freeze drier dry 48h, obtains white
Color powder；
(4) by above-mentioned white powder, in nitrogen atmosphere, it is calcined to 3h at 500 DEG C, heating rate is 4 DEG C/min,
Obtain nitrogen boron codope porous carbon materials.
Embodiment 11:
(1) 0.4g para hydroxybenzene boric acid is dissolved in 4mL deionized water, magnetic agitation 1h, is uniformly mixed, is obtained para hydroxybenzene
Boric acid solution；
(2) under magnetic stirring, while by 8mL cyanamide and 4mL para hydroxybenzene boric acid solution it is added dropwise to 12mL deionization
In water, magnetic agitation 1h is uniformly mixed, obtains mixed solution；
(3) it by mixed solution obtained above, is rapidly frozen with liquid nitrogen, is put into freeze drier dry 48h, obtains white
Color powder；
(4) by above-mentioned white powder, in argon atmosphere, it is calcined to 3h at 500 DEG C, heating rate is 2 DEG C/min,
Obtain nitrogen boron codope porous carbon materials.
Embodiment 12:
(1) 0.4g para hydroxybenzene boric acid is dissolved in 4mL deionized water, magnetic agitation 1h, is uniformly mixed, is obtained para hydroxybenzene
Boric acid solution；
(2) under magnetic stirring, while by 8mL cyanamide and 4mL para hydroxybenzene boric acid solution it is added dropwise to 12mL deionization
In water, magnetic agitation 1h is uniformly mixed, obtains mixed solution；
(3) it by mixed solution obtained above, is rapidly frozen with liquid nitrogen, is put into freeze drier dry 48h, obtains white
Color powder；
(4) by above-mentioned white powder, in argon atmosphere, it is calcined to 3h at 500 DEG C, heating rate is 5 DEG C/min,
Obtain nitrogen boron codope porous carbon materials.
Preparation condition summary sheet
In order to further verify the mesoporous presence of material, nitrogen boron codope porous carbon that above-described embodiment is prepared
Material has carried out the test of nitrogen De contamination, the nitrogen De contamination for the nitrogen boron codope porous carbon materials that wherein embodiment 1 is prepared
Test curve and pore-size distribution are as depicted in figs. 1 and 2.The object proposed according to International Union of Pure and Applied Chemistry (IUPAC)
Adsorption isotherm classification is managed, isotherm plots shown in Fig. 1 move towards, the specific surface area that is calculated about 62.3m similar to II type2g-1.The presence of B-H loop, which also indicates that, in Fig. 3 has meso-hole structure abundant in material.CxNyBJH (the Barret- of B material
Joyner-Halenda) method pore-size distribution is as shown in Figure 2, it can be seen that material internal it is widely distributed a large amount of hole, Kong Zhi
Diameter is differed from 3.17nm to 45.31nm.The pore size data further illustrates that the sample is meso-hole structure (macropore range 2nm-
50nm)。
The nitrogen boron codope porous carbon materials and acetylene black, polyvinylidene fluoride that above-described embodiment is prepared
(polyvinylidene difluoride, abbreviation PVDF) is mixed according to the mass ratio of 8:1:1 and is ground uniformly, with N- methyl
Pyrrolidones (NMP) makees solvent, and mixture is uniformly coated on the copper foil for having weighed good quality, is then placed in 120 DEG C true
Empty drying box is stayed overnight.Using ethylene carbonate (EC) and dimethyl carbonate (DMC) binary electrolyte, (EC/DMC volume ratio is 1:1)
And lithium hexafluoro phosphate (LiPF6) electrolytic salt commercial lithium battery electrolytes, battery snap specification be CR2032, lithium piece is done negative
The nitrogen boron codope porous carbon materials of pole, preparation do anode.Battery assembly from the bottom to top sequence: bottom buckle, sodium piece, diaphragm, electrode
Piece electrolyte, gasket, elastic slice, is buckled greatly, then is encapsulated with button cell sealing machine, is taken out from glove box, has been carried out energy release and has been surveyed
Examination.
Fig. 3 shows the test result after the application of 1 material prepared of embodiment.As can be seen that widely distributed in material
Duct is internal after assembled battery to will be filled with electrolyte solution, accelerates Li+Transport, to show excellent electrochemistry
Can, in the current density of 100mA/g, release energy 553mAh/g, after 200 circle of circulation, capacity almost without decline, and cost compared with
Low, synthesis process is simple, provides possibility for the practical application after it in lithium ion battery material.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Within the technical scope of the present disclosure, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should all be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection of claims
Subject to range.
Claims (6)
1. a kind of preparation method of nitrogen boron codope porous carbon composite, which is characterized in that the preparation method includes:
Appropriate para hydroxybenzene boric acid is dissolved in deionized water with 1:10 mass ratio, stirring 1h is uniformly mixed it, obtains to hydroxyl
Base phenyl boric acid solution；
The appropriate amount of deionized water persistently stirred is added according to volume ratio 1:(0.2-5) for cyanamide and para hydroxybenzene boric acid solution
In, stirring 1-5h is uniformly mixed it, obtains mixed solution；
It is rapidly frozen mixed solution to form frozen material with liquid nitrogen, and frozen material is put into freeze drier dry 36~60h,
Obtain white powder；
Inert gas is passed through in heating furnace and forms inert atmosphere, and white powder is put into the heating furnace, makes described add
Hot stove carries out temperature programming and white powder is calcined in the heating furnace, obtains nitrogen boron codope porous carbon composite wood
Material.
2. the preparation method of nitrogen boron codope porous carbon composite according to claim 1, which is characterized in that described right
Hydroxy benzenes boric acid concentration is at least 97%.
3. the preparation method of nitrogen boron codope porous carbon composite according to claim 1, which is characterized in that the ammonia
Base cyanogen concentration is at least 93%.
4. the preparation method of nitrogen boron codope porous carbon composite according to claim 3, which is characterized in that the ammonia
Base cyanogen and the total volume of the para hydroxybenzene boric acid solution and deionized water volume ratio are 1:(0.5~2).
5. the preparation method of nitrogen boron codope porous carbon composite according to claim 1, which is characterized in that described lazy
Property gas be nitrogen or argon gas.
6. the preparation method of nitrogen boron codope porous carbon composite according to claim 1, is characterized in that, the heating
Furnace programmed rate is 2-5 DEG C/min, and calcination temperature is 400~800 DEG C, and 0.5~4h of calcination time.
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