CN107697902A - A kind of double-doped class graphene nano carbon material of boron nitrogen and preparation method and application - Google Patents
A kind of double-doped class graphene nano carbon material of boron nitrogen and preparation method and application Download PDFInfo
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Abstract
The invention provides double-doped class graphene nano carbon material of a kind of boron nitrogen and preparation method and application, the preparation method comprises the following steps：(1) crystalline flake graphite, is subjected to ball milling under air atmosphere, obtains nitrogenous class graphene carbon material；(2), the nitrogenous class graphene carbon material is well mixed with boron-containing compound, calcined under inert atmosphere, after calcining terminates, obtains the double-doped class graphene nano carbon material of the boron nitrogen.The double-doped class graphene nano carbon material of the boron nitrogen that the present invention is prepared is used as the electrode material of ultracapacitor, understand that it has excellent electrochemical energy storage effect by test, higher specific capacitance characteristic, circulating effect is preferable, capacitance conservation rate is expected to apply in actual production use more than 75% under high current.
Description
Technical field
The present invention relates to double-doped class graphene nano carbon material of a kind of boron nitrogen and preparation method and application, belongs to modification and receives
Rice carbon material preparing technical field.
Background technology
Energy problem has had become the major issue for concerning survival and development of mankind, right with the development of human society
It is growing day by day in the demand of clean energy resource, thus promote the development of New Energy Industry.Ultracapacitor is as a kind of new
Green energy storage device, has the energy density higher than traditional capacitor and a power density higher than battery, and its can keep compared with
Long service life cycle and quick charge efficiency.But at present for the more ripe Ni-MH battery of technique and lithium battery,
Ultracapacitor still has the problem of capacity is relatively low, and it is used alone as independent current source can not meet daily life needs.
Thus the key of development ultracapacitor is the specific capacitance for how improving capacitor.Carbon material is with its Stability Analysis of Structures, price
The advantages of cheap, turns into preferable electrode material substitute, but itself redox active is poor, relies primarily on to electric charge
Suction-operated stores electric charge, and specific capacity is relatively low.Thus, carbon material is modified in itself to strengthen its redox active, increased
Big its specific surface area and increase pore structure have very great help for the specific capacity for improving carbon material.
The content of the invention
In order to solve the shortcomings that above-mentioned and deficiency, it is an object of the invention to provide a kind of double-doped class graphene nano of boron nitrogen
The preparation method of carbon material.
The present invention also aims to provide the preparation method preparation by the double-doped class graphene nano carbon material of above-mentioned boron nitrogen
The obtained double-doped class graphene nano carbon material of boron nitrogen.
The present invention also aims to provide the double-doped class graphene nano carbon material of above-mentioned boron nitrogen as super capacitor electrode
The application of pole.
To reach above-mentioned purpose, the present invention provides a kind of preparation method of the double-doped class graphene nano carbon material of boron nitrogen, its
Comprise the following steps：
(1) crystalline flake graphite, is subjected to ball milling under air atmosphere, obtains nitrogenous class graphene carbon material；
(2), the nitrogenous class graphene carbon material is well mixed with boron-containing compound, forged under inert atmosphere
Burn, after calcining terminates, obtain the double-doped class graphene nano carbon material of the boron nitrogen.
According to specific embodiments of the present invention, in the preparation method, it is preferable that the nitrogenous class graphene carbon material
Mass ratio between boron-containing compound is 1:3-6, more preferably 1:5.
According to specific embodiments of the present invention, in the preparation method, the nitrogen member in the nitrogenous class graphene carbon material
Element comes from the nitrogen in air.
According to specific embodiments of the present invention, it is preferable that the preparation method also includes using the nitrogenous class of low concentration acid elution
The operation of graphene carbon material.Wherein, can be removed using the nitrogenous class graphene carbon material of low concentration acid elution may wherein deposit
Metal impurities, and those skilled in the art can need reasonable selection low concentration sour according to operation, of the invention specific
In embodiment, low concentration acid used is 1M hydrochloric acid (HCl).
According to specific embodiments of the present invention, in the preparation method, it is preferable that a diameter of 3- of steel ball used in ball milling
The mass ratio of 6mm, more preferably 5mm, crystalline flake graphite and steel ball is 1-2:50.Wherein, used in the specific embodiment of the invention
A diameter of 5mm steel ball ball-milling treatment crystalline flake graphite, ball-milling treatment can be directly by steel balls and graphite point by screening after terminating
From subsequently again with the i.e. removable metal residual that may be present of low concentration acid treatment.
According to specific embodiments of the present invention, in the preparation method, it is preferable that the rotational speed of ball-mill is 500-
1500rpm, Ball-milling Time 12-48h.
According to specific embodiments of the present invention, in the preparation method, it is preferable that the boron-containing compound includes boron
Any of acid, diboron trioxide and sodium borohydride.Nitrogenous class graphene carbon material is under the conditions of high-temperature calcination, its nitrogenous official
Meeting Auto-decomposition can be rolled into a ball, and after introducing boron source (boron-containing compound), nitrogen is effectively retained, and (boron element plays in this process
The effect of fixed nitrogen), doping efficiency is higher.
According to specific embodiments of the present invention, in the preparation method, the inert atmosphere includes nitrogen and/or argon
Gas.
According to specific embodiments of the present invention, in the preparation method, it is preferable that the calcining heat is 700-900
DEG C, calcination time 3-5h, more preferably 4h.
According to specific embodiments of the present invention, the preparation method also includes calcining products therefrom being down to room temperature, then with 80
The operation of DEG C hot deionized water washing and filtering.
Present invention also offers the boron nitrogen that the preparation method of the double-doped class graphene nano carbon material of above-mentioned boron nitrogen is prepared
Double-doped class graphene nano carbon material.
According to specific embodiments of the present invention, it is preferable that the matter of boron in the double-doped class graphene nano carbon material of boron nitrogen
Amount content is 0.6-1.92%, and the mass content of nitrogen is 1.91-2.86%.
According to specific embodiments of the present invention, it is preferable that the ratio surface of the double-doped class graphene nano carbon material of boron nitrogen
Product is 700-800m2/ g, pore diameter distribution scope are 2-10nm.
Present invention also offers application of the double-doped class graphene nano carbon material of above-mentioned boron nitrogen as electrode of super capacitor.
The present invention uses crystalline flake graphite and boron-containing compound to be brought it about for raw material by easy ball milling and high-temperature process
The double-doped class graphene nano carbon material of boron nitrogen is prepared in chemical conversion.The material has advantages below：
1st, the specific surface area and pore structure of the material are effectively increased by ball-milling treatment, i.e. the present invention is prepared
The double-doped class graphene nano carbon material of boron nitrogen has larger specific surface area, and shows loose structure, and pore passage structure is distributed
It is homogeneous；
2nd, heteroatomic doping is realized by high-temperature process, adds the surface functional group (nitrogen-containing functional group of the material
And boracic functional group) content；
3rd, using crystalline flake graphite as raw material, its is cheap, and preparation technology is simple, can be mass-produced.The material is used as
The electrode material of ultracapacitor, understand that it has an excellent electrochemical energy storage effect by test, higher specific capacitance characteristic,
Circulating effect is preferable, and capacitance conservation rate is expected to apply in actual production use more than 75% under high current.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture for the double-doped class graphene nano carbon material of boron nitrogen that the embodiment of the present invention 1 is prepared；
Fig. 2 is that the BET for the double-doped class graphene nano carbon material of boron nitrogen that the embodiment of the present invention 1 is prepared schemes, interior in Fig. 2
Embedding figure is its graph of pore diameter distribution；
Fig. 3 is the XRD for the double-doped class graphene nano carbon material of boron nitrogen that the embodiment of the present invention 1 is prepared；
Fig. 4 is the Raman figures for the double-doped class graphene nano carbon material of boron nitrogen that the embodiment of the present invention 1 is prepared；
Fig. 5 is the XPS figures for the double-doped class graphene nano carbon material of boron nitrogen that the embodiment of the present invention 1 is prepared；
Fig. 6 is the double-doped class graphene nano carbon material of boron nitrogen that is prepared of the embodiment of the present invention 1 in 6M KOH solutions
Specific volume spirogram under different current densities, the embedded figure in Fig. 6 be current density be 0.25A/g and 100A/g under discharge and recharge it is bent
Line；
Fig. 7 is the double-doped class graphene nano carbon material of boron nitrogen that is prepared of the embodiment of the present invention 1 in 6M KOH solutions,
Circulating effect figure under 25A/g.
Embodiment
In order to which technical characteristic, purpose and the beneficial effect of the present invention is more clearly understood, in conjunction with detail below
Embodiment to technical scheme carry out it is described further below, but it is not intended that to the present invention can practical range limit
It is fixed.
Embodiment 1
A kind of preparation method of the double-doped class graphene nano carbon material of boron nitrogen is present embodiments provided, it includes following step
Suddenly：
5g crystalline flake graphites are placed in the ball grinder containing 250g steel balls (under air atmosphere), and ball grinder is fixed on ball
On grinding machine, rotational speed of ball-mill is set as 750rpm, after handling 48h, collects sample, washing and filtering is carried out with 1M hydrochloric acid (HCl), remove
The metal impurities that may wherein contain, obtaining nitrogenous class graphene carbon material, (as can be seen from Figure 5 crystalline flake graphite is in air gas
Ball milling introduces nitrogen wherein really in atmosphere)；
Products therefrom 1g in step (1) is taken, with 5g boric acid (H3BO3) be transferred in quartz boat after mixing, it is positioned over tube furnace
In boiler tube, under argon gas (Ar) protective effect, system temperature is risen to 900 DEG C simultaneously by room temperature with 5 DEG C/min heating rate
4h is kept, treats that temperature is down to room temperature, by product with 80 DEG C of hot deionized water washing and filterings, you can obtain the double-doped class graphite of boron nitrogen
Alkene nano-carbon material.
The double-doped class graphene nano carbon material of boron nitrogen that embodiment 1 is prepared carry out respectively transmission electron microscope, BET,
XRD, Raman, XPS analysis, wherein, transmission electron microscope picture, BET figures, the XRD of the double-doped class graphene nano carbon material of the boron nitrogen
Figure, Raman figures, XPS figures difference are as Figure 1-5；
From figure 1 it appears that the material that embodiment 1 is prepared has layer structure, class graphene-structured is presented；
As can be seen from Figure 2, the specific surface area of crystalline flake graphite raw material is 11.43m2/ g, the boron nitrogen that embodiment 1 prepares gained are double-doped
The specific surface area of class graphene nano material is 802.35m2/ g, it is seen that its specific surface area significantly increases after the treatment；By hole
Footpath distribution map is understood, the double-doped class graphene nano material of boron nitrogen that is porose, and passing through processing preparation gained is free from raw material
Even aperture distribution, 2-10nm is distributed in, focuses primarily upon 3.6nm or so；
From figure 3, it can be seen that the double-doped class graphene nano material of the boron nitrogen that embodiment 1 is prepared is in 2 θ=26 °
Nearby there are two obvious peaks with 44 °, it corresponds to (002) and (100) peak of hexagonal structure graphitic carbon respectively；
There are three obvious peaks in Fig. 4, correspond to the D peaks, G peaks and 2D peaks of graphite-structure respectively, because defect is more,
2900cm-1Nearby there are more obvious D+G peaks；
This it appears that the presence at N peaks and B peaks from Fig. 5, it is computed learning B, the mass content of N element is respectively
1.92% and 2.86%.
Embodiment 2
A kind of preparation method of the double-doped class graphene nano carbon material of boron nitrogen is present embodiments provided, it includes following step
Suddenly：
10g crystalline flake graphites are placed in the ball grinder containing 250g steel balls (under air atmosphere), and ball grinder is fixed on
On ball mill, rotational speed of ball-mill is set as 900rpm, after handling 36h, is collected sample, is carried out washing and filtering with 1M hydrochloric acid (HCl), remove
The metal impurities that may wherein contain are removed, obtain nitrogenous class graphene carbon material；
Products therefrom 1g in step (1) is taken, with 5g diboron trioxides (B2O3) be transferred in quartz boat after mixing, it is positioned over
In tube furnace boiler tube, under argon gas (Ar) protective effect, rise to 800 DEG C with 5 DEG C/min heating rate and keep 4h, treat temperature
Degree is down to room temperature, by product with 80 DEG C of hot deionized water washing and filterings, you can obtain the double-doped class graphene nano carbon materials of boron nitrogen
Expect, B, the mass content of N element are respectively 1.39% and 2.30% in the material.
Embodiment 3
A kind of preparation method of the double-doped class graphene nano carbon material of boron nitrogen is present embodiments provided, it includes following step
Suddenly：
5g crystalline flake graphites are placed in the ball grinder containing 250g steel balls (under air atmosphere), and ball grinder is fixed on ball
On grinding machine, rotational speed of ball-mill is set as 500rpm, after handling 48h, collects sample, washing and filtering is carried out with 1M hydrochloric acid (HCl), remove
The metal impurities that may wherein contain, nitrogenous class graphene carbon material is obtained, the N element mass content of the material is 3.3%；
Products therefrom 1g in step (1) is taken, with 5g sodium borohydrides (NaBH4) be transferred in quartz boat after mixing, it is positioned over
In tube furnace boiler tube, under argon gas (Ar) protective effect, rise to 700 DEG C with 5 DEG C/min heating rate and keep 4h, treat temperature
Degree is down to room temperature, by product with 80 DEG C of hot deionized water washing and filterings, you can obtain the double-doped class graphene nano carbon materials of boron nitrogen
Material, the specific surface area of the material is about 700m2/ g, B, the mass content of N element are respectively 0.60% and 1.91%.
From embodiment 1-3, with the rise of calcining heat, the double-doped class stone of preparation-obtained boron nitrogen in embodiment
Boron nitrogen content in black alkene nano-carbon material has raised, and compared to the nitrating class graphene carbon material obtained after ball milling
(nitrogen content 3.3%), the nitrogen content of the preparation-obtained double-doped class graphene of boron nitrogen has declined in embodiment 1-3, this
Illustrate that nitrogen-containing functional group is decomposed in calcination process, and then cause nitrogen content to be lost in, and pass through and improve calcining heat increasing
Add the activity of boron atom so that Boron contents increase and further serve the effect of fixed nitrogen.
Embodiment 4
A kind of preparation method of the double-doped class graphene nano carbon material of boron nitrogen is present embodiments provided, it includes following step
Suddenly：
10g crystalline flake graphites are placed in the ball grinder containing 250g steel balls (under air atmosphere), and ball grinder is fixed on
On ball mill, rotational speed of ball-mill is set as 1500rpm, after handling 12h, collects sample, washing and filtering is carried out with 1M hydrochloric acid (HCl),
Remove the metal impurities that may wherein contain；
Products therefrom 1g in step (1) is taken, with 5g boric acid (H3BO3) be transferred in quartz boat after mixing, it is positioned over tube furnace
In boiler tube, under argon gas (Ar) protective effect, rise to 750 DEG C with 5 DEG C/min heating rate and keep 4h, treat that temperature is down to
Room temperature, by product with 80 DEG C of hot deionized water washing and filterings, you can obtain the double-doped class graphene nano carbon material of boron nitrogen.
Embodiment 5
A kind of preparation method of the double-doped class graphene nano carbon material of boron nitrogen is present embodiments provided, it includes following step
Suddenly：
5g crystalline flake graphites are placed in the ball grinder containing 250g steel balls (under air atmosphere), and ball grinder is fixed on ball
On grinding machine, rotational speed of ball-mill is set as 1200rpm, after handling 24h, is collected sample, is carried out washing and filtering with 1M hydrochloric acid (HCl), remove
Remove the metal impurities that may wherein contain；
Products therefrom 1g in step (1) is taken, with 5g diboron trioxides (B2O3) be transferred in quartz boat after mixing, it is positioned over
In tube furnace boiler tube, under argon gas (Ar) protective effect, rise to 850 DEG C with 5 DEG C/min heating rate and keep 4h, treat temperature
Degree is down to room temperature, by product with 80 DEG C of hot deionized water washing and filterings, you can obtain the double-doped class graphene nano carbon materials of boron nitrogen
Material.
Application examples
The double-doped class graphene nano carbon material of boron nitrogen that the embodiment of the present invention is prepared is used as the electricity of ultracapacitor
Pole material, its specific capacity in 6M KOH solutions under different current densities is measured, test result is as shown in Figure 6；Measure simultaneously
Its charging and discharging curve in the case where current density is respectively 0.25A/g and 100A/g, specific charging and discharging curve are shown in embedded in Fig. 6
Figure；From fig. 6 it can be seen that under 0.25A/g current density, its capacity can reach 255F/g, when current density increases
During to 100A/g, its capacity is the 78% of 199F/g, about initial capacity, this explanation double-doped class of boron nitrogen under high current density
The charge and discharge effect of graphene nano carbon material is fine；
In addition, also measuring the electrode material in the application example in 6M KOH solutions, current density is that effect is circulated under 25A/g
Fruit, test result as shown in Figure 7, it can be seen from figure 7 that after the circulation of 20000 circles, still can by its capacitance conservation rate
Enough reach 93%, it is excellent that this shows that the double-doped class graphene nano carbon material of the boron nitrogen can show under the conditions of big charging current
Performance, it is especially suitable for practical application.
Claims (10)
1. a kind of preparation method of the double-doped class graphene nano carbon material of boron nitrogen, it comprises the following steps：
(1) crystalline flake graphite, is subjected to ball milling under air atmosphere, obtains nitrogenous class graphene carbon material；
(2), the nitrogenous class graphene carbon material is well mixed with boron-containing compound, is calcined, forged under inert atmosphere
After sintering beam, the double-doped class graphene nano carbon material of the boron nitrogen is obtained.
2. preparation method according to claim 1, it is characterised in that this method also includes nitrogenous using low concentration acid elution
The operation of class graphene carbon material.
3. preparation method according to claim 1, it is characterised in that a diameter of 3-6mm of steel ball used in ball milling, be preferably
The mass ratio of 5mm, crystalline flake graphite and steel ball is 1-2:50.
4. the preparation method according to claim 1 or 3, it is characterised in that the rotational speed of ball-mill is 500-1500rpm, ball
Consume time as 12-48h.
5. preparation method according to claim 1, it is characterised in that the boron-containing compound includes boric acid, three oxidations two
Any of boron and sodium borohydride.
6. preparation method according to claim 1, it is characterised in that the nitrogenous class graphene carbon material and boracic chemical combination
Mass ratio between thing is 1:3-6, preferably 1:5.
7. preparation method according to claim 1, it is characterised in that the calcining heat is 700-900 DEG C, calcination time
For 3-5h, preferably 4h.
8. the boron nitrogen that the preparation method of the double-doped class graphene nano carbon material of any one of the claim 1-7 boron nitrogen is prepared
Double-doped class graphene nano carbon material；
Preferably, the mass content of boron is 0.6-1.92% in the double-doped class graphene nano carbon material of the boron nitrogen, the quality of nitrogen
Content is 1.91-2.86%.
9. the double-doped class graphene nano carbon material of boron nitrogen according to claim 8, it is characterised in that the ratio surface of the material
Product is 700-800m2/ g, pore diameter distribution scope are 2-10nm.
10. application of the double-doped class graphene nano carbon material of the boron nitrogen of claim 8 or 9 as electrode of super capacitor.
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Cited By (4)
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| CN108529590A (en) * | 2018-04-23 | 2018-09-14 | 江汉大学 | A kind of nitrogen boron codope carbon material and preparation method thereof |
| CN111377446A (en) * | 2020-04-14 | 2020-07-07 | 安徽工业大学 | Preparation method of nitrogen and boron double-doped humic acid based porous carbon material with high thermal stability |
| CN114426272A (en) * | 2020-09-24 | 2022-05-03 | 中国石油化工股份有限公司 | Sulfur-boron doped carbon material, platinum-carbon catalyst, and preparation methods and applications thereof |
| CN115849367A (en) * | 2022-12-21 | 2023-03-28 | 中国五矿集团(黑龙江)石墨产业有限公司 | Sodium-ion battery negative electrode material based on natural graphite raw material, preparation method of sodium-ion battery negative electrode material and sodium-ion battery |
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