CN107804837A - A kind of preparation method of 3D nanometers chip architecture N doping class graphene - Google Patents
A kind of preparation method of 3D nanometers chip architecture N doping class graphene Download PDFInfo
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- CN107804837A CN107804837A CN201711101241.5A CN201711101241A CN107804837A CN 107804837 A CN107804837 A CN 107804837A CN 201711101241 A CN201711101241 A CN 201711101241A CN 107804837 A CN107804837 A CN 107804837A
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- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The invention belongs to field prepared by grapheme material, more particularly to a kind of preparation method of 3D nanometers chip architecture N doping class graphene, this method to comprise the following steps：（1）, by vegetable oil and nitrogen source with mass ratio 1：1 20 are mixed, grind 5 120 min, obtain mixture A, and the nitrogen source is mixture more than one or both of urea, melamine, cyanamid dimerization；Described vegetable oil is mixture more than one or both of corn oil, soybean oil, rapeseed oil, sunflower oil, peanut oil；（2）, by step（1）In obtained mixture A be placed in tube furnace under nitrogen atmosphere, being warming up to 800 1400 DEG C with 18 DEG C/min heating rate carries out calcining 2 10 h, obtains product.Time saving simple, the suitable volume production of preparation method operation of the present invention, and institute's prepared material is in 3D stereochemical structures, has the characteristics that specific surface area is big, pore volume is big.
Description
Technical field
The invention belongs to field prepared by grapheme material, more particularly to a kind of 3D nanometers chip architecture N doping class graphene
Preparation method.
Background technology
Since 2004 are found, its research boom continues to this day graphene.Graphene is peeled off from graphite material
Out, the two dimensional crystal for the only one layer of atomic thickness being made up of carbon atom.It is a kind of bidimensional being made up of carbon hexatomic ring
(2D) cycle honeycomb lattice structure, can be warped into zero dimension（0D）Fullerene or be curled into the CNT of one-dimensional (1D)
Or the graphite of three-dimensional (3D) is stacked to, therefore graphene is the elementary cell for forming other graphite materials.Graphene is special
Physicalchemical structure makes it have many innovation performances, and it has good intensity, thermal conductivity and electric conductivity, while its basic knot
Structure unit is most stable of benzene hexatomic ring in organic material, and therefore, graphene is presently the most preferable two-dimension nano materials.
Class grapheme material is a kind of quasi- two-dimensional system material with graphene-structured, and class graphene-structured is that handle has
The methods of being peeled off similar to the inorganic compound of graphite laminate crystal structure by physics is obtained by chemical synthesis process
Monatomic (molecule) thickness degree or monatomic (molecule) layer of multilayer be accumulated to the quasi- two-dimensional nanostructures of several nanometer thickness
System.Class grapheme material due to the structure similar with graphene and its innovation performance, absorption, catalysis, Aero-Space,
New energy field of batteries etc. has great application prospect, has become the focus studied after graphene
The conventional preparation method of class grapheme material has：（1）" from top to bottom " method；（2 " from bottom to top " methods." from top to bottom " method
The class graphene-structured compound of individual layer or several layers of molecular thickness is mainly prepared by stripping method.This method can obtain quality
High, the class graphene of excellent performance, but this method takes time and effort, and can not meet the requirement of volume production." from bottom to top " method is
Refer to the two-dimensional nano class graphite for synthesizing individual layer or several layers of atoms (molecule) thickness by atom (molecule) by chemical synthesis process
Alkene structure." from bottom to top " method controllability it is stronger, can volume production, but operational control is complicated, and synthesis cost is high, and purity, photoelectricity
Performance etc. is also than the poor performance of stripping method.Therefore, how a kind of simple and effective class graphene material for preparing suitable volume production
Material has great importance.
The content of the invention
The present invention is solves cumbersome, waste of materials in above-mentioned N doping class grapheme material preparation process, during preparation
Between the technical problem such as long and a kind of preparation method of simple and effective 3D nanometers chip architecture N doping class graphene is provided.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of preparation method of 3D nanometers chip architecture N doping class graphene, this method comprise the following steps：
（1）, by vegetable oil and nitrogen source with mass ratio 1：1-20 is mixed, is ground 5-120 min, obtains mixture A, the nitrogen
Source is mixture more than one or both of urea, melamine, cyanamid dimerization；Described vegetable oil is corn oil, greatly
Mixture more than one or both of soya-bean oil, rapeseed oil, sunflower oil, peanut oil；
（2）, by step（1）In obtained mixture A be placed in tube furnace under nitrogen atmosphere, with 1-8 DEG C/min heating speed
Rate is warming up to 800-1400 DEG C and carries out calcining 2-10 h, obtains a kind of N doping class graphene material with 3D nanometer chip architectures
Material.
Time saving simple, the suitable volume production of preparation method operation of the present invention, and institute's prepared material is in 3D stereochemical structures, is had than surface
The features such as product is big, pore volume is big.Simultaneously as used carbon source is renewable carbon source, meet the principle of sustainable development, and
And due to N doping, improve the performance of graphene.
The present invention uses vegetable oil and nitrogen source, and grinding relief vegetable oil is thoroughly mixed to form tightly packed with nitrogen source.Will
To vegetable oil and the mixture of nitrogen source be placed in and calcine under nitrogen atmosphere, because vegetable oil and nitrogen source are pyrolyzed stripping at high temperature
From mutual doping reaction so that product is obtained after calcining and forms nitrating class graphene composite structure.Simultaneously as material is forged
It is in 3D stereochemical structures after burning, that is, has obtained a kind of 3D nanometers chip architecture N doping class grapheme material.Calcining heat is higher, gained
The class grapheme material degree of graphitization arrived is higher, and pore volume is also bigger.And by changing the shape of container and mixture, also
Macroscopic view, which can be obtained, has the 3D nanometer chip architecture N doping class grapheme materials of given shape.
Preferably, described vegetable oil and the mass ratio of nitrogen source are 1：1-20.
Preferably, step（1）In vegetable oil and nitrogen source mass ratio be 1： 1；Described nitrogen source is urea；It is described
Vegetable oil be corn oil.
Preferably, step（1）In vegetable oil and nitrogen source mass ratio be 1：2；Described nitrogen source is cyanamid dimerization；Institute
The vegetable oil stated is rapeseed oil.
Preferably, step（1）In vegetable oil and nitrogen source mass ratio be 1：4；Described nitrogen source is melamine；Institute
The vegetable oil stated is soybean oil.
Preferably, step（1）In vegetable oil and nitrogen source mass ratio be 1：6；Described nitrogen source be melamine and
The mixture of urea, both mass ratioes are 1:1；Described vegetable oil is sunflower oil.
Preferably, step（1）In vegetable oil and nitrogen source mass ratio be 1：8；Described nitrogen source be cyanamid dimerization and
The mixture of melamine, both mass ratioes are 1:1；Described vegetable oil is the miscella of soybean oil and peanut oil, Liang Zhezhi
Amount is than being 1:1.
Preferably, step（1）In vegetable oil and nitrogen source mass ratio be 1：10；Described nitrogen source is urea and dimerization
The mixture of cyanamide, both mass ratioes are 1:1；Described vegetable oil is the miscella of corn oil and rapeseed oil, both mass ratioes
For 1:1.
Preferably, step（1）In vegetable oil and nitrogen source mass ratio be 1：15；Described nitrogen source be melamine and
The mixture of urea, both mass ratioes are 1:1；Described vegetable oil is the miscella of soybean oil and sunflower oil, both quality
Than for 1:1.
Preferably, step（1）In vegetable oil and nitrogen source mass ratio be 1：20；Described nitrogen source be cyanamid dimerization and
The mixture of melamine, both mass ratioes are 1:1；Described vegetable oil is the mixing of soybean oil, rapeseed oil and sunflower oil
Oil, three's mass ratio are 1:1:1.
The beneficial effects of the invention are as follows：The preparation method of the 3D nanometer chip architecture N doping class graphenes of the present invention is abundant
Direct high temperature pyrolysis after mixed vegetable oil and organic compounds containing nitrogen, shorten the preparation time of material.Except this, because nitrogen is mixed
It is miscellaneous, the content of amino in material is improved, improves the performance of class graphene.The N doping class graphene that the present invention obtains is compound
Material, in 3D stereochemical structures, and there is larger specific surface area and pore volume, it is than surface 150-600 m2/ g, aperture 2-8 nm,
Pore volume 2-7.5 cm3/ g, and the degree of graphitization of material can regulate and control, in biological medicine, catalysis, Aero-Space, new energy
There is great application prospect in source battery field etc..This method has simple to operate, and production cost is low, and controllability is stronger,
The features such as being adapted to volume production.Compared to common graphite alkene, the 3D nanometer chip architecture N doping class graphene materials of the final gained of the present invention
Material not only has larger specific surface area, and into 3D stereochemical structures, beneficial to practical application.
Brief description of the drawings
Fig. 1 is the photo of the different macroshape 3D nanometers chip architecture N doping class graphenes of the present invention；
Fig. 2 is the stereoscan photograph of 3D nanometers chip architecture N doping class graphene of the present invention.
Embodiment
Below by specific embodiment, technical scheme is described in further detail.It should be appreciated that this hair
Bright implementation is not limited to the following examples, and any formal accommodation and/or change made to the present invention will all fall
Enter the scope of the present invention.
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, used equipment and raw material etc.
It is commercially available or commonly used in the art.Method in following embodiments, it is the normal of this area unless otherwise instructed
Rule method.
Embodiment 1
A kind of preparation method of 3D nanometers chip architecture N doping class grapheme material, is specifically comprised the following steps：
（1）, in mass ratio calculate, i.e. vegetable oil：Nitrogen source is 1：1,2g vegetable oil is mixed with 2g nitrogen sources, and be sufficiently mixed grinding
5 min, obtained mixture is transferred in quartz boat；
Described nitrogen source is urea；
Described vegetable oil is corn oil.
（2）, by step（1）In the obtained mixture of the vegetable oil containing nitrogen source be placed in tube furnace under nitrogen atmosphere,
900 DEG C are warming up to 2 DEG C/min heating rate and carries out calcining 2h, obtain 3D nanometer chip architecture N doping class grapheme materials.
3D nanometer chip architecture nitrogen using Bei Shide 3H-2000PS4 types specific surface areas and Porosimetry to above-mentioned gained
Doping class grapheme material is measured, and its specific surface area is 176 m2/ g, aperture are 2.8 nm, and pore volume is 3.15 cm3/g。
Embodiment 2
A kind of preparation method of the class grapheme material of 3D structures N doping, is specifically comprised the following steps：
（1）, in mass ratio calculate, i.e. vegetable oil：Nitrogen source is 1：2,2g vegetable oil is mixed with 4g nitrogen sources, and be sufficiently mixed grinding
15 min, obtained mixture is transferred in quartz boat；
Described nitrogen source is cyanamid dimerization；
Described vegetable oil is rapeseed oil.
（2）, by step（1）In the obtained mixture of the vegetable oil containing nitrogen source be placed in tube furnace under nitrogen atmosphere,
800 DEG C are warming up to 3 DEG C/min heating rate to carry out calcining 8 h, obtain the class grapheme material of 3D structure N dopings.
3D nanometer chip architecture nitrogen using Bei Shide 3H-2000PS4 types specific surface areas and Porosimetry to above-mentioned gained
Doping class grapheme material is measured, and its specific surface area is 255 m2/ g, aperture are 4.4 nm, and pore volume is 2.89 cm3/g。
Embodiment 3
A kind of preparation method of the class grapheme material of 3D structures N doping, is specifically comprised the following steps：
（1）, in mass ratio calculate, i.e. vegetable oil：Nitrogen source is 1：4,2g vegetable oil is mixed with 8g nitrogen sources, and be sufficiently mixed grinding
30 min, obtained mixture is transferred in quartz boat；
Described nitrogen source is melamine；
Described vegetable oil is soybean oil.
（2）, by step（1）In the obtained mixture of the vegetable oil containing nitrogen source be placed in tube furnace under nitrogen atmosphere,
1000 DEG C are warming up to 3 DEG C/min heating rate and carries out calcining 2h, obtain the class grapheme material of 3D structure N dopings.
3D nanometer chip architecture nitrogen using Bei Shide 3H-2000PS4 types specific surface areas and Porosimetry to above-mentioned gained
Doping class grapheme material is measured, and its specific surface area is 291 m2/ g, aperture are 5.5 nm, and pore volume is 5.16 cm3/g。
Embodiment 4
A kind of preparation method of the class grapheme material of 3D structures N doping, is specifically comprised the following steps：
（1）, in mass ratio calculate, i.e. vegetable oil：Nitrogen source is 1：6,2g vegetable oil is mixed with 12g nitrogen sources, and be sufficiently mixed and grind
60 min are ground, obtained mixture is transferred in quartz boat；
Described nitrogen source is the mixture of melamine and urea, and both mass ratioes are 1:1；
Described vegetable oil is sunflower oil.
（2）, by step（1）In the obtained mixture of the vegetable oil containing nitrogen source be placed in tube furnace under nitrogen atmosphere,
1200 DEG C are warming up to 4 DEG C/min heating rate and carries out calcining 5h, obtain the class grapheme material of 3D structure N dopings.
3D nanometer chip architecture nitrogen using Bei Shide 3H-2000PS4 types specific surface areas and Porosimetry to above-mentioned gained
Doping class grapheme material is measured, and its specific surface area is 383 m2/ g, aperture are 4.8 nm, and pore volume is 6.46 cm3/g。
Embodiment 5
A kind of preparation method of the class grapheme material of 3D structures N doping, is specifically comprised the following steps：
（1）, in mass ratio calculate, i.e. vegetable oil：Nitrogen source is 1：8,2g vegetable oil is mixed with 16g nitrogen sources, and be sufficiently mixed and grind
60 min are ground, obtained mixture is transferred in quartz boat；
Described nitrogen source is the mixture of cyanamid dimerization and melamine, and both mass ratioes are 1:1；
Described vegetable oil is the miscella of soybean oil and peanut oil, and both mass ratioes are 1:1.
（2）, by step（1）In the obtained mixture of the vegetable oil containing nitrogen source be placed in tube furnace under nitrogen atmosphere,
1100 DEG C are warming up to 5 DEG C/min heating rate and carries out calcining 2h, obtain the class grapheme material of 3D structure N dopings.
3D nanometer chip architecture nitrogen using Bei Shide 3H-2000PS4 types specific surface areas and Porosimetry to above-mentioned gained
Doping class grapheme material is measured, and its specific surface area is 573 m2/ g, aperture are 7.6 nm, and pore volume is 7.34 cm3/g。
Embodiment 6
A kind of preparation method of the class grapheme material of 3D structures N doping, is specifically comprised the following steps：
（1）, in mass ratio calculate, i.e. vegetable oil：Nitrogen source is 1：10,2g vegetable oil is mixed with 20g nitrogen sources, and be sufficiently mixed and grind
90 min are ground, obtained mixture is transferred in quartz boat；
Described nitrogen source is the mixture of urea and cyanamid dimerization, and both mass ratioes are 1:1;
Described vegetable oil is the miscella of corn oil and rapeseed oil, and both mass ratioes are 1:1.
（2）, by step（1）In the obtained mixture of the vegetable oil containing nitrogen source be placed in tube furnace under nitrogen atmosphere,
1300 DEG C are warming up to 1.5 DEG C/min heating rate and carries out calcining 6h, obtain the class grapheme material of 3D structure N dopings.
3D nanometer chip architecture nitrogen using Bei Shide 3H-2000PS4 types specific surface areas and Porosimetry to above-mentioned gained
Doping class grapheme material is measured, and its specific surface area is 481 m2/ g, aperture are 6.56 nm, and pore volume is 4.11 cm3/
g。
Embodiment 7
A kind of preparation method of the class grapheme material of 3D structures N doping, is specifically comprised the following steps：
（1）, in mass ratio calculate, i.e. vegetable oil：Nitrogen source is 1：15,2g vegetable oil is mixed with 30g nitrogen sources, and be sufficiently mixed and grind
120 min are ground, obtained mixture is transferred in quartz boat；
Described nitrogen source is the mixture of melamine and urea, and both mass ratioes are 1:1；
Described vegetable oil is the miscella of soybean oil and sunflower oil, and both mass ratioes are 1:1.
（2）, by step（1）In the obtained mixture of the vegetable oil containing nitrogen source be placed in tube furnace under nitrogen atmosphere,
1400 DEG C are warming up to 2 DEG C/min heating rate and carries out calcining 3h, obtain the class grapheme material of 3D structure N dopings.
3D nanometer chip architecture nitrogen using Bei Shide 3H-2000PS4 types specific surface areas and Porosimetry to above-mentioned gained
Doping class grapheme material is measured, and its specific surface area is 593 m2/ g, aperture are 7.88 nm, and pore volume is 3.32 cm3/
g。
Embodiment 8
A kind of preparation method of the class grapheme material of 3D structures N doping, is specifically comprised the following steps：
（1）, in mass ratio calculate, i.e. vegetable oil：Nitrogen source is 1：20,2g vegetable oil is mixed with 40g nitrogen sources, and be sufficiently mixed and grind
120 min are ground, obtained mixture is transferred in quartz boat；
Described nitrogen source is the mixture of cyanamid dimerization and melamine, and both mass ratioes are 1:1；
Described vegetable oil is the miscella of soybean oil, rapeseed oil and sunflower oil, and three's mass ratio is 1:1:1.
（2）, by step（1）In the obtained mixture of the vegetable oil containing nitrogen source be placed in tube furnace under nitrogen atmosphere,
1400 DEG C are warming up to 2 DEG C/min heating rate and carries out calcining 5h, obtain the class grapheme material of 3D structure N dopings.
3D nanometer chip architecture nitrogen using Bei Shide 3H-2000PS4 types specific surface areas and Porosimetry to above-mentioned gained
Doping class grapheme material is measured, and its specific surface area is 399 m2/ g, aperture 5.91nm, pore volume are 3.97 cm3/g。
The photo of 3D nanometers chip architecture N doping class graphene of the present invention is shown in Fig. 1, before filling mixing when being calcined by changing
The container shapes of object, can obtain macroscopic view has given shape 3D class graphenes.3D nanometers chip architecture N doping class of the present invention
The stereoscan photograph of graphene is shown in Fig. 2.In summary, 3D nanometers chip architecture N doping class grapheme material produced by the present invention
Specific surface area be 150-600 m2/ g, aperture 2-8 nm, pore volume 2-7.5 cm3/ g, illustrate the preparation method gained of the present invention
3D nanometer chip architecture N dopings class grapheme material specific surface area and pore volume it is larger, pore structure is uniform, and material
Degree of graphitization can regulate and control, it can be applied to biological medicine, electrochemistry and CO2Capture is with being catalyzed recycling etc..
Embodiment described above is a kind of preferable scheme of the present invention, not the present invention is made any formal
Limitation, there are other variants and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (10)
1. a kind of preparation method of 3D nanometers chip architecture N doping class graphene, it is characterised in that this method comprises the following steps：
（1）, by vegetable oil and nitrogen source with mass ratio 1：1-1000 is mixed, is ground 0.5-1.5h, obtains mixture A, described
Nitrogen source is mixture more than one or both of urea, melamine, cyanamid dimerization, single poly cyanamid；Described vegetable oil
For mixture more than one or both of corn oil, soybean oil, rapeseed oil, sunflower oil, peanut oil；
（2）, by step（1）In obtained mixture A be placed in tube furnace under nitrogen atmosphere, with 1-5 DEG C/min heating speed
Rate is warming up to 800-1400 DEG C and carries out calcining 2-6h, obtains a kind of N doping class grapheme material with 3D nanometer chip architectures.
2. preparation method according to claim 1, it is characterised in that：Described vegetable oil and the mass ratio of nitrogen source are 1：1-
20。
3. preparation method according to claim 1, it is characterised in that：Step（1）In vegetable oil and nitrogen source mass ratio
For 1： 1；Described nitrogen source is urea；Described vegetable oil is corn oil.
4. preparation method according to claim 1, it is characterised in that：Step（1）In vegetable oil and nitrogen source mass ratio
For 1：2；Described nitrogen source is cyanamid dimerization；Described vegetable oil is rapeseed oil.
5. preparation method according to claim 1, it is characterised in that：Step（1）In vegetable oil and nitrogen source mass ratio
For 1：4；Described nitrogen source is melamine；Described vegetable oil is soybean oil.
6. preparation method according to claim 1, it is characterised in that：Step（1）In vegetable oil and nitrogen source mass ratio
For 1：6；Described nitrogen source is the mixture of melamine and urea, and both mass ratioes are 1:1；Described vegetable oil is sunflower seeds
Oil.
7. preparation method according to claim 1, it is characterised in that：Step（1）In vegetable oil and nitrogen source mass ratio
For 1：8；Described nitrogen source is the mixture of cyanamid dimerization and melamine, and both mass ratioes are 1:1；Described vegetable oil is big
The miscella of soya-bean oil and peanut oil, both mass ratioes are 1:1.
8. preparation method according to claim 1, it is characterised in that：Step（1）In vegetable oil and nitrogen source mass ratio
For 1：10；Described nitrogen source is the mixture of urea and cyanamid dimerization, and both mass ratioes are 1:1；Described vegetable oil is corn
The miscella of oil and rapeseed oil, both mass ratioes are 1:1.
9. preparation method according to claim 1, it is characterised in that：Step（1）In vegetable oil and nitrogen source mass ratio
For 1：15；Described nitrogen source is the mixture of melamine and urea, and both mass ratioes are 1:1；Described vegetable oil is soybean
The miscella of oil and sunflower oil, both mass ratioes are 1:1.
10. preparation method according to claim 1, it is characterised in that：Step（1）In vegetable oil and nitrogen source mass ratio
For 1：20；Described nitrogen source is the mixture of cyanamid dimerization and melamine, and both mass ratioes are 1:1；Described vegetable oil is
The miscella of soybean oil, rapeseed oil and sunflower oil, three's mass ratio are 1:1:1.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108975315A (en) * | 2018-07-28 | 2018-12-11 | 嘉兴学院 | The preparation method of the grapheme material of three-dimensional manometer lamellar structure |
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| CN103771405A (en) * | 2014-01-22 | 2014-05-07 | 绍兴文理学院 | Preparation method for nano multiporous graphene material functionalized by strongly acidic ionic liquid |
| CN104229789A (en) * | 2014-09-25 | 2014-12-24 | 上海交通大学 | Preparation method of nitrogen-doped graphene |
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| CN103771405A (en) * | 2014-01-22 | 2014-05-07 | 绍兴文理学院 | Preparation method for nano multiporous graphene material functionalized by strongly acidic ionic liquid |
| CN104229789A (en) * | 2014-09-25 | 2014-12-24 | 上海交通大学 | Preparation method of nitrogen-doped graphene |
| CN104760951A (en) * | 2015-04-09 | 2015-07-08 | 新疆大学 | Preparation method of nitrogen-doped graphene |
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