CN108264037B - Three-dimensional porous nitrogen-doped graphene answers the preparation method of material and nitrogen-doped graphene - Google Patents
Three-dimensional porous nitrogen-doped graphene answers the preparation method of material and nitrogen-doped graphene Download PDFInfo
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- CN108264037B CN108264037B CN201810116559.9A CN201810116559A CN108264037B CN 108264037 B CN108264037 B CN 108264037B CN 201810116559 A CN201810116559 A CN 201810116559A CN 108264037 B CN108264037 B CN 108264037B
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Abstract
A kind of three-dimensional porous nitrogen-doped graphene composite material and nitrogen-doped graphene preparation method, belong to function nano Material Field.Specific steps are as follows: nine water ferric nitrates and polyvinylpyrrolidone are dissolved respectively and are made into mixed solution in deionized water, after ultrasonic agitation, resulting mixed solution is placed in air dry oven and is completely dried rear grind into powder；The obtained powder of grinding is transferred to again and is placed in tube furnace in inert protective atmosphere heating and thermal insulation in crucible to get the three-dimensional porous nitrogen-doped graphene composite material nano-particle modified to cementite.The nano-particle modified three-dimensional porous graphene composite material of cementite is placed in heating water bath in strong acid, is cooled to room temperature to solution, filters, cleans, is centrifuged, then be freeze-dried and obtain three-dimensional porous nitrogen-doped graphene.The present invention is with short production cycle, at low cost, and repeatability is strong and can be prepared on a large scale, and has important reference function to the preparation of graphene-based composite material, also has broad prospect of application in fields such as energy storage, catalysis.
Description
Technical field
The invention belongs to function nano Material Fields, and in particular to a kind of three-dimensional porous nitrogen-doped graphene composite material and
The large-scale preparation method of nitrogen-doped graphene.
Background technique
Carbon-based material is a kind of important traditional material, because its excellent mechanics, optics, electricity, calorifics, etc. performances form
For one of research direction important in the fields such as chemistry, material, physics.And arc lighting device, communication have been widely used in it
The fields such as device, electrical equipment, energy storage and electrocatalysis material.However, the performance of traditional carbon material is with development in science and technology
It is unable to satisfy practical application request, therefore the exploitation of novel carbon-based material causes the great attention of scientists.
Graphene as a kind of novel carbon-based material, due to its very excellent performance solar battery, sensor,
Extensive research has been obtained in the fields such as elctro-catalyst and metal ion battery.The conventional method of synthesizing graphite alkene has oxidation also
Former method, chemical vapour deposition technique, electrolysis method etc., but the usual yield of graphene of these methods preparation is smaller and at high cost；And
In the graphene film of two-dimentional stacking form in electro-catalysis, there are limitations for the application in the fields such as electromagnetic wave absorbent material.In recent years,
High Temperature Chemical Foaming method synthesis three-dimensional grapheme based composites have become a kind of effective and novel synthetic technology.?
There are some three-dimensional grapheme materials to prepare by this method, but three-dimensional porous nitrogen-doped graphene based composites there is not yet
Document report.Graphene introduces nitrogen atom doping, can improve the electro catalytic activity of catalyst.Therefore, spy is controllably prepared
Shape the nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of cementite of looks and high-specific surface area and three-dimensional more
Hole nitrogen-doped graphene has extremely important theoretical and practical significance for the development of graphene-based composite material.Through document
Investigation, have no the high Temperature Chemical Foaming method nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of preparation cementite and
The report of three-dimensional porous nitrogen-doped graphene.
Summary of the invention
The present invention provides a kind of simple, efficient, low cost, the three-dimensional porous nitrogen-doped graphene composite material of prepare with scale
And nitrogen-doped graphene preparation method.
A kind of preparation method of three-dimensional porous nitrogen-doped graphene composite material, it is characterised in that include the following steps:
1) nine water ferric nitrates and polyvinylpyrrolidone are dissolved respectively and is made into mixed solution in deionized water, ultrasound is stirred
3~15min is mixed, wherein nine water ferric nitrates and polyvinylpyrrolidone mass ratio are (1.0~3.0): 1.
2) mixed solution is placed in heat preservation in convection oven until being completely dried, then pulverized；
3) ground powder is transferred in crucible, then by crucible be placed in tube furnace in inert protective atmosphere with
The heating rate of 1~20 DEG C/min is heated to 500~900 DEG C, and keeps the temperature 1~3h, after tube furnace is cooled to room temperature, collects black
The nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of color foam-like product, as cementite.
Further, nine water ferric nitrates and polyvinylpyrrolidone mass ratio are (1.0~3.0) in the step 1): 1,
It is preferred that (1.5~2.0): 1.
Further, the drying temperature in the step 2) is 60~80 DEG C.
Further, high pure nitrogen or high-purity argon gas can be used in the inert protective atmosphere in the step 3).Prepared
The bore dia of three-dimensional porous graphene composite material is 10~15 μm or so, and what is obtained is three-dimensional graphite skeletal support
Fe3A small number of layer nitrogen-doped graphenes of C@C Core-shell Structure Nanoparticles modification, Fe3C nano particle size is 10~30nm.
A kind of preparation method of three-dimensional porous nitrogen-doped graphene, specific preparation step are as follows:
1) the nano-particle modified three-dimensional porous graphene composite material of above-mentioned cementite is placed in strong acid 70~90
4~6h of heating water bath at DEG C.
2) it is cooled to room temperature to solution, filters black powder, cleaned, be centrifuged with deionized water, then be freeze-dried to obtain
To three-dimensional porous graphene.
Further, hydrochloric acid, nitric acid or its mixed acid may be selected in the strong acid in the step 1), and concentration is 1~2mol/
L。
A kind of three-dimensional porous nitrogen-doped graphene composite material proposed by the invention and nitrogen-doped graphene preparation method,
There is not yet document report.Preparation method is simple, and method is novel, with short production cycle, can prepare with scale.And the iron nano-particle that is carbonized
The three-dimensional porous nitrogen-doped graphene composite material and three-dimensional porous nitrogen-doped graphene of modification are due to special three-dimensional knot
Structure and nanoscale Fe3The modification of C C core-shell structure, can not only greatly improve its specific surface area, and can inhibit graphene
It stacks, it is made to be hopeful to be widely used in catalysis and field of batteries.
This method has the advantage that
1) method is simple to operation, at low cost, can prepare with scale, the three-dimensional porous nitrogen-doped graphene base prepared
Material morphology is kept, and has directive significance to the synthesis regulation of other relevant graphene-based materials.
2) by the accurate control to reactant content and heating rate, different foaming can be prepared in a relatively short period of time
Degree and the nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of the cementite of different-shape.
3) three-dimensional porous nitrogen-doped graphene is accessed by mild acidification etching energy, without destroying its three-dimensional structure.
Detailed description of the invention
Fig. 1 is the nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of cementite prepared by the present invention
XRD spectrum.
Fig. 2 is the nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of cementite prepared by the present invention
FESEM photo.
Fig. 3 is the nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of cementite prepared by the present invention
AFM photo, illustration are that line sweeps curve.
Fig. 4 is the nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of cementite prepared by the present invention
TEM photo.
Fig. 5 is the nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of cementite prepared by the present invention
XPS-N1s map, the presence at the peak show that N atom is successfully entrained in graphene base body, graphite known to after the fitting of N1s swarming
There are the nitrogen of type in 3, i.e. pyridine nitrogen in alkene, graphite nitrogen and pyrroles's nitrogen.
Fig. 6 is the XRD spectrum of three-dimensional porous nitrogen-doped graphene prepared by the present invention.
Fig. 7 is the FESEM photo of three-dimensional porous nitrogen-doped graphene prepared by the present invention.
Specific embodiment
Embodiment one
1:1 in mass ratio weighs polyvinylpyrrolidonepowder powder and nine water ferric nitrates, by nine water ferric nitrates and polyethylene pyrrole
Pyrrolidone dissolves respectively is made into mixed solution ultrasonic agitation 10min in deionized water, and mixed solution is then placed in air blast and is done
80 DEG C of heat preservations are until be completely dried, then the product after drying is ground into powder and powder is transferred in crucible, earthenware in dry case
Crucible is placed in tube furnace in N2700 DEG C are heated to the heating rate of 5 DEG C/min in atmosphere, keeps the temperature 1h, after tube furnace is cooling
Black foam shape product is collected, the nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of cementite is obtained.
Embodiment two
1:1.5 in mass ratio weighs polyvinylpyrrolidonepowder powder and nine water ferric nitrates, by nine water ferric nitrates and polyethylene
Pyrrolidones dissolves respectively is made into mixed solution ultrasonic agitation 10min in deionized water, and mixed solution is then placed in air blast
80 DEG C of heat preservations are until be completely dried in drying box, then the product after drying is ground into powder and powder is transferred in crucible,
Crucible is placed in tube furnace in N2700 DEG C are heated to the heating rate of 5 DEG C/min in atmosphere, keeps the temperature 1h, it is cooling to tube furnace
Black foam shape product is collected afterwards, obtains the nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of cementite.
Embodiment three
1:2.0 in mass ratio weighs polyvinylpyrrolidonepowder powder and nine water ferric nitrates, by nine water ferric nitrates and polyethylene
Pyrrolidones dissolves respectively is made into mixed solution ultrasonic agitation 10min in deionized water, and mixed solution is then placed in air blast
80 DEG C of heat preservations are until be completely dried in drying box, then the product after drying is ground into powder and powder is transferred in crucible,
Crucible is placed in tube furnace in N2700 DEG C are heated to the heating rate of 5 DEG C/min in atmosphere, keeps the temperature 1h, it is cooling to tube furnace
Black foam shape product is collected afterwards, obtains the nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of cementite.
Example IV
1:1.5 in mass ratio weighs polyvinylpyrrolidonepowder powder and nine water ferric nitrates, by nine water ferric nitrates and polyethylene
Pyrrolidones dissolves respectively is made into mixed solution ultrasonic agitation 10min in deionized water, and mixed solution is then placed in air blast
80 DEG C of heat preservations are until be completely dried in drying box, then the product after drying is ground into powder and powder is transferred in crucible,
Crucible is placed in tube furnace in N2700 DEG C are heated to the heating rate of 1 DEG C/min in atmosphere, keeps the temperature 1h, it is cooling to tube furnace
Black foam shape product is collected afterwards, obtains the nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of cementite.
Embodiment five
1:1.5 in mass ratio weighs polyvinylpyrrolidonepowder powder and nine water ferric nitrates, by nine water ferric nitrates and polyethylene
Pyrrolidones dissolves respectively is made into mixed solution ultrasonic agitation 10min in deionized water, and mixed solution is then placed in air blast
80 DEG C of heat preservations are until be completely dried in drying box, then the product after drying is ground into powder and powder is transferred in crucible,
Crucible is placed in tube furnace in N2700 DEG C are heated to the heating rate of 10 DEG C/min in atmosphere, keeps the temperature 1h, it is cooling to tube furnace
Black foam shape product is collected afterwards, obtains the nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of cementite.
Embodiment six
1:1.5 in mass ratio weighs polyvinylpyrrolidonepowder powder and nine water ferric nitrates, by nine water ferric nitrates and polyethylene
Pyrrolidones dissolves respectively is made into mixed solution ultrasonic agitation 10min in deionized water, and mixed solution is then placed in air blast
80 DEG C of heat preservations are until be completely dried in drying box, then the product after drying is ground into powder and powder is transferred in crucible,
Crucible is placed in tube furnace in N2700 DEG C are heated to the heating rate of 10 DEG C/min in atmosphere, keeps the temperature 1h, it is cooling to tube furnace
Black foam shape product is collected afterwards, obtains the nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of cementite.It will
The nano-particle modified three-dimensional porous graphene composite material of cementite is placed in 2mol/L hydrochloric acid and 2mol/L nitric acid mixed acid (body
Product than 3:1) at 70 DEG C heating water bath 6h, be cooled to room temperature to solution, filter black powder, cleaned with deionized water, from
The heart, then it is freeze-dried to obtain three-dimensional porous graphene.
The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof, the ordinary skill people of fields
Member should be appreciated that can be with modifications or equivalent substitutions are made to specific embodiments of the invention referring to above-described embodiment, these
Applying within pending claims without departing from any modification of spirit and scope of the invention or equivalent replacement.
Claims (6)
1. a kind of preparation method of three-dimensional porous nitrogen-doped graphene composite material, it is characterised in that include the following steps:
A. nine water ferric nitrates and polyvinylpyrrolidone are dissolved respectively and is made into mixed solution in deionized water, ultrasonic agitation 3
~15min, wherein nine water ferric nitrates and polyvinylpyrrolidone mass ratio are (1.0~3.0): 1；
B. mixed solution is placed in heat preservation in convection oven until being completely dried, then pulverized；
C. ground powder is transferred in crucible, then crucible is placed in tube furnace in inert protective atmosphere with 1~
The heating rate of 20 DEG C/min is heated to 500~900 DEG C, and keeps the temperature 1~3h, after tube furnace is cooled to room temperature, collects black
The nano-particle modified three-dimensional porous nitrogen-doped graphene composite material of foam-like product, as cementite.
2. the preparation method of three-dimensional porous nitrogen-doped graphene composite material according to claim 1, it is characterised in that institute
Stating nine water ferric nitrates and polyvinylpyrrolidone mass ratio in step a is (1.5~2.0): 1.
3. the preparation method of three-dimensional porous nitrogen-doped graphene composite material according to claim 1, it is characterised in that institute
Stating the drying temperature in step b is 60~80 DEG C.
4. the preparation method of three-dimensional porous nitrogen-doped graphene composite material according to claim 1, it is characterised in that institute
The inert protective atmosphere in step c is stated using high pure nitrogen or high-purity argon gas；Prepared three-dimensional porous graphene composite material
Aperture be 10~15 μm, that obtain is the Fe of three-dimensional graphite skeletal support3The minority of C@C Core-shell Structure Nanoparticles modification
Layer nitrogen-doped graphene, Fe3C nano particle size is 15~30nm.
5. a kind of three-dimensional more using the preparation method preparation of three-dimensional porous nitrogen-doped graphene composite material described in claim 1
The method of hole nitrogen-doped graphene, it is characterised in that specific preparation step are as follows:
1) the nano-particle modified three-dimensional porous graphene composite material of cementite is placed in strong acid the water-bath at 70~90 DEG C
Heat 4~6h；
2) it is cooled to room temperature to solution, filters black powder, cleaned, be centrifuged with deionized water, then be freeze-dried and obtain three-dimensional
Porous nitrogen-doped graphene.
6. the method according to claim 5 for preparing three-dimensional porous nitrogen-doped graphene, it is characterised in that the step 1)
In strong acid to select hydrochloric acid, nitric acid or its mixed acid, and concentration be 1~2mol/L.
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| CN110124703B (en) * | 2019-05-14 | 2020-10-13 | 北京科技大学 | Preparation method of iron phosphide-loaded graphene foam composite material |
| CN110404567B (en) * | 2019-08-27 | 2022-04-22 | 中国人民解放军国防科技大学 | Photocatalytic energy conversion material and preparation method and application thereof |
| CN110828819B (en) * | 2019-10-28 | 2020-11-27 | 北京科技大学 | Pyrrhotite type iron sulfide negative electrode material for potassium ion battery and preparation method thereof |
| CN110828796B (en) * | 2019-10-29 | 2020-11-27 | 北京科技大学 | Yolk shell structure potassium ion battery negative electrode material and preparation method thereof |
| CN111170310B (en) * | 2020-01-15 | 2022-02-25 | 北京科技大学 | Three-dimensional graphene/carbon nanotube composite material and preparation method thereof |
| CN113690413B (en) * | 2021-07-09 | 2023-03-14 | 郑州大学 | Preparation method of high-efficiency sodium-ion battery cathode carbon composite material |
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